CN107459354A - High transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof - Google Patents
High transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof Download PDFInfo
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Abstract
The present invention provides at least one of high-purity aluminum oxynitride and yittrium oxide, magnesia, titanium oxide, silica, zinc oxide compound high transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof, using the high-purity composite nitrogen alumina powder of nanoscale and noresidue binding agent, noresidue surfactant, noresidue lubricant, noresidue plasticizer is kneaded, pelletized after mixing, the particle made is put into injection (mo(u)lding) machine again and is injection moulded, dumping sintering processes are finally carried out, that is, obtain high transmittance High Purity Nitrogen alumina transparent ceramic.The present invention has the advantages of high-purity high transmittance high intensity, not only technique and equipment are simple by the present invention, cost is low, high income, energy consumption is low, and production efficiency is high, it is adapted to industrialized production, and the tiny controllable aluminum oxynitride crystalline ceramics of steady quality, crystal grain can be obtained, process of the present invention without Environment pollution, be a kind of new low cost, steady quality high transmittance High Purity Nitrogen alumina transparent ceramic preparation method.
Description
Technical field
The invention belongs to material preparation process technical field, and in particular to a kind of transparent pottery of high-purity aluminum oxynitride of high transmittance
Porcelain and preparation method thereof.
Background technology
It has been ceramic material since R.L.Coble in 1962 is reported successfully be prepared for transparent alumina ceramic material first
Material opens new application field.This material not only has the preferably transparency, and corrosion-resistant, can work at high temperature under high pressure
To make, also many other unrivaled properties of material, such as intensity are high, dielectric properties are excellent, low conductivity, highly thermally conductive property,
So gradually obtained in fields such as lighting engineering, optics, extraordinary instrument manufacturing, wireless electron technology and high-temperature technologies increasingly extensive
Application.In recent years, in the world many countries, the especially U.S., Japan, Britain, Russia, France etc. to transparent ceramic material
Make substantial amounts of research work, successively have developed Al2O3、Y2O3、MgO、CaO、TiO2、ThO2、ZrO2Made pottery Deng oxidic transparent
Porcelain and AlN, ZnS, ZnSe, MgF2、CaF2Etc. Non-oxide Transparent Ceramics.
Chinese patent 201410459441.8 provides a kind of MULTILAYER COMPOSITE YAG crystalline ceramics, transparent using MULTILAYER COMPOSITE
Ceramic material, fluorescent material Ce and Pr are introduced respectively in upper and lower transparent ceramic layer, using raising SiO2The intermediate layer of content, use
One-step calcination method prepares MULTILAYER COMPOSITE crystalline ceramics, improves traditional gold-tinted Ce:The luminous spy of YAG crystalline ceramics LED lamps
Property, make the blue light that blue light excitation source is sent that there is more preferable colour temperature and colour developing transmitted through the white light sent after YAG crystalline ceramics
Index.
Chinese patent 201410790363.X provides a kind of preparation method of ZnS crystalline ceramics, and it is comprised the following steps that：
Thioacetamide and zinc chloride are dissolved in deionized water and are made into mixed solution as mother liquor, will using positive titration method
Hydrochloric acid and ammoniacal liquor mixed precipitation agent solution are added drop-wise in mother liquor, while heating stirring, after the pH value for adjusting solution, are staticly settled；
By centrifuging out sediment, deposit is then cleaned, obtains presoma sediment；The presoma drying precipitate that will be obtained
Powder sieving afterwards；The powder of sieving is pre-processed with tube furnace, then powder is subjected to vacuum heating-press sintering, ZnS is made
Crystalline ceramics.
Chinese patent 201410773181.1 provides a kind of crystalline ceramics of white light LEDs, by the component of following number
Calcining composition：70-80 part mullite powders, 80-100 part titanium dioxides, 50-75 part silica flours, 100-120 part alukalins, 15-
20 parts of zirconium dioxides, 8-10 part ytterbium oxides, 5-8 part lanthanas, 5-7 part sodium metasilicate, the nano oxidized holmium of 6-10 parts, the oxidation of 5-8 parts
Dysprosium, 8-10 part calcium carbonate.
Chinese patent 201410156302.8 provides a kind of aluminum oxynitride crystalline ceramics and preparation method thereof, the nitrogen oxygen
Change aluminium crystalline ceramics, be to ooze technology by ion thermal expansion to penetrate into Mg on aluminum oxynitride crystalline ceramics surface2+, the infiltration Mg2+'s
The thickness for oozing magnesium layer is 50~600 μm.Methods described includes：Using aluminum oxynitride crystalline ceramics as base material, with Mg compound
Source is oozed as expansion, base material is wrapped in into expansion oozes in source, makes Mg by the ion thermal expansion technology of oozing2+Substitute Al3+, that is, obtain the nitrogen
Alumina transparent ceramic.
Chinese patent 201010137522.8 provides a kind of preparation method of MgAlON crystalline ceramics.The transparent potteries of MgAlON
The pressureless sintering preparation method of porcelain, it is characterised in that it comprises the following steps：1）The preparation of MgAlON transparent ceramic powders；2）Press
95~99.9wt% of MgAlON transparent ceramic powders, 0.1~5wt% of fluoride, mixing are scattered in absolute ethyl alcohol, and ball milling obtains
Slurry B；3）Slurry B is dried, obtains mixture B；4）By mixture B at normal temperatures using axially molding is compressing, passes through again
After isostatic cool pressing compacting, biscuit of ceramics is obtained；5）Sintering, obtains MgAlON crystalline ceramics.MgAlON prepared by the invention is transparent
Ceramics, without high consistency can be obtained by techniques such as HIP sinterings（＞ 99.5%）With excellent optical property,
Thickness is that best straight line transmitance of the 2mm plate material in 0.25~6 μ m wavelength range is more than 70%.
Chinese patent 201210339362.4 provides a kind of Lanthanum gadolinium zirconate transparent ceramic material and preparation method thereof, described
The chemical composition of Lanthanum gadolinium zirconate transparent ceramic material is La2-xGdxZr2O7, wherein 0 ＜ x ＜ 2, preferably 0.4≤x≤1.6.The hair
The visible light transmissivity of the Lanthanum gadolinium zirconate transparent ceramic material of bright offer is high, while sintered density is high, can meet to visit in information
The application requirement in the field such as survey, laser medium, high-temperature window and high index of refraction camera lens, scintillator matrix.
Chinese patent 200910195846.4 provides a kind of preparation method of the yttrium oxide transparent ceramic of high optical quality,
Belong to crystalline ceramics preparation field.Preparation method comprises the following steps：With the high-purity Y of business2O3Powder is raw material, ZrO2For sintering
Auxiliary agent, using zirconia ball as abrasive media, add mixing and ball milling 3-30h after absolute ethyl alcohol；Polypropylene is added in above-mentioned powder
Barbiturates dispersant, is configured to Y2O3Water-based slurry, using porous resin moulds or the slip casting of porous alumina ceramic mould into
Type；The finally pressureless sintering in vacuum or hydrogen atmosphere stove, obtains the yttrium oxide transparent ceramic of high optical quality.Y thick 2mm2O3
Crystalline ceramics transmitance at 1100nm is up to 81.3%.
Chinese patent 201010611540.5 provides a kind of preparation method of zirconic acid yttrium transparent ceramics, belongs to crystalline ceramics
Field.Comprise the following steps：1）It is prepared by powder：Zirconic acid yttrium nano-powder is prepared using combustion method；2）Shaping：By step 1）Gained
It is biscuit that zirconic acid yttrium nano-powder is dry-pressing formed under 5~20MPa, then gained biscuit is carried out in 180~230MPa cold etc. quiet
Pressure processing；3）Sintering：By step 2）Prior to 1000~1400 DEG C 2~4h of pre-burning of sample after processing, then under vacuum
4~10h is sintered at 1800~1900 DEG C；4）Annealing heat-treats：By step 3）Sample after sintering in air atmosphere in
2~10h is incubated at 1400~1600 DEG C, annealing heat-treats is carried out, obtains zirconic acid yttrium transparent ceramics.The crystalline ceramics is in visible ray
The maximum linear transmitance of scope is more than 65%.
Chinese patent 201110194521.1 provides a kind of preparation method of LiAlON crystalline ceramics, belongs to crystalline ceramics
Field of material preparation.The pressureless sintering preparation method of LiAlON crystalline ceramics, it is characterised in that it comprises the following steps：1）Will
LiAlON transparent ceramic powders are dried, and obtain powder A；2）Powder A is compressing using axially molding at normal temperatures, then pass through
After the compacting of 100~250MPa isostatic cool pressings, biscuit of ceramics is obtained；3）Biscuit of ceramics is placed in crucible, crucible is placed in be burnt without pressure
In freezing of a furnace, protected with flowing nitrogen, 1~20 DEG C/min heating rate is heated to 1750~1975 DEG C, 5~30h of insulation, nature
LiAlON sintered bodies are obtained after cooling；Sintered body obtains LiAlON crystalline ceramics after grinding, polishing.This method is advantageous to
Control sample forms and without that can obtain high relative density by techniques such as HIP sinterings（＞ 99.5%）, add
Work is after thickness is 2mm plate materials, in the range of 0.25~6 μm of light wave, to have preferable straight line transmittance.
Chinese patent 201310491922.2 provides one kind and prepares aluminum oxynitride crystalline ceramics using gel casting forming
Method, including：（1）After aluminum oxynitride powder, dispersant and absolute ethyl alcohol ball milling mixing water resistant agent will be added to carry out hydration-resisting
Dried after processing, sieving obtains the aluminum oxynitride powder handled through hydration-resisting, aluminum oxynitride powder, dispersant and the hydration-resisting
The mass ratio of agent is 100：（0.1~5）：（0.1~5）；（2）By the aluminum oxynitride powder of hydration-resisting processing, water-soluble isobutene
Compound of birdsing of the same feather flock together is mixed to prepare water-based slurry with water, wherein aluminum oxynitride powder, the water-soluble isobutylene type of hydration-resisting processing
The mass ratio of polymer and water is（10~80）：（0.1~5）：100；（3）Mould will be injected after the water-based slurry vacuum degassing
Middle progress obtains biscuit from gel solidification and is dried；And（4）Dried biscuit is subjected to pre-burning and pressureless sintering system
Obtain the aluminum oxynitride crystalline ceramics.
Chinese patent 200710013607.3 provides a kind of preparation method of transparent aluminum oxynitride ceramic, including raw material
Proportioning, blank forming and sintering process, it is characterised in that：By weight than the Al for 80~95%2O3AlN with 5~20% is mixed
Close, separately add sintering aid by the 0.1~9% of its mixture weight, sintering aid is by Al powder, Y2O3Formed with MgO, Huo Zheyou
Y2O3Formed with MgO, the addition respectively formed is Al2O3With the 0.05~3% of AlN mixture weights, dried after ball milling, so
It is first dry-pressing formed afterwards, then acquisition base substrate is pressed into isostatic pressed, elder generation's vacuum is warming up to 800~1200 DEG C of insulations when base substrate is burnt till
0.5~3 hour, then pass to nitrogen and reach normal pressure, then be warming up to 1750~1900 DEG C and be incubated 0.5~8 hour, that is, obtain saturating
Bright aluminum oxynitride ceramic material.For this method using once normal pressure-sintered technique, technique is simple, and firing temperature is low, will to equipment
Ask not high, the transparent material of acquisition ultra-violet (UV) band transmitance more than 90%, the transmitance of near infrared region reach 50% with
On, relative density reaches more than the 99% of solid density.
Chinese patent 201410308279.X provides a kind of nano aluminium oxide enhancing aluminum oxynitride ceramic and its preparation side
Method, belong to nanometer admixture field of ceramic preparation technology.The invention is right by being defined to each phase component content proportioning in raw material
Sintering temperature, pressure and soaking time are defined, so as to prepare the aluminum oxynitride ceramic of nano aluminium oxide admixture；Nano oxygen
The addition for changing aluminium focuses mostly at grain boundaries, forms Grain boundary pinning effect, the obstruction ability of On Crack Propagation is very high, material
Bending strength and fracture transmitance are high.
Prior art is studied only for low-purity aluminum oxynitride forming technique, is not sintered for high-purity fine grain
High-strength technology is studied, narrower so as to the application surface of product, without the strength characteristics for really playing aluminum oxynitride material.
The content of the invention
Used to solve prior art in industrial and civilian product high transmittance High Purity Nitrogen alumina transparent ceramic
In can not meet the situation of requirement, the invention provides a kind of brand-new high transmittance High Purity Nitrogen alumina transparent ceramic and its system
Preparation Method.The shortcomings that it is an object of the invention to overcome prior art, and it is adjustable to provide a kind of straight line transmittance, it is cheap
Aluminum oxynitride crystalline ceramics, there is provided in high-purity aluminum oxynitride and yittrium oxide, magnesia, titanium oxide, silica, zinc oxide extremely
Few a kind of compound high transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof, using the high-purity compound nitrogen oxidation of nanoscale
Aluminium powder and noresidue binding agent, noresidue surfactant, noresidue lubricant, noresidue plasticizer are kneaded, have been kneaded
Pelletized after finishing, then the particle made be put into injection (mo(u)lding) machine and is injection moulded, finally carry out dumping sintering processes,
Obtain high transmittance High Purity Nitrogen alumina transparent ceramic.The present invention has the advantages of high-purity high transmittance high intensity, the present invention
Not only technique and equipment are simple, and cost is low, and high income, energy consumption is low, and production efficiency is high, are adapted to industrialized production, and can obtain
Steady quality, the tiny controllable aluminum oxynitride crystalline ceramics of crystal grain, process of the present invention are a kind of new low without Environment pollution
Cost, steady quality high transmittance High Purity Nitrogen alumina transparent ceramic preparation method.
Aluminum oxynitride crystalline ceramics relative density of the present invention be 95% ~ 99.9%, host element purity be 99.5% ~
99.999%, bending strength is 1200 ~ 3000MPa, and crystallite dimension is 0.1 ~ 20 micron, and Vickers hardness is HV2000 ~ 20000, directly
Line transmitance is more than 70%.
Preferably, the relative density of described high transmittance High Purity Nitrogen alumina transparent ceramic is 97% ~ 99%.
Preferably, the host element purity of described high transmittance High Purity Nitrogen alumina transparent ceramic is 99.9% ~ 99.999%.
Preferably, the bending strength of described high transmittance High Purity Nitrogen alumina transparent ceramic is 1400 ~ 2500MPa.
Preferably, the crystallite dimension of described high transmittance High Purity Nitrogen alumina transparent ceramic is 0.2 ~ 2 micron.
Preferably, the Vickers hardness of described high transmittance High Purity Nitrogen alumina transparent ceramic is HV2500 ~ 16000.
Preferably, the straight line transmittance of described high transmittance High Purity Nitrogen alumina transparent ceramic is more than 80%.
The host element of high transmittance High Purity Nitrogen alumina transparent ceramic of the present invention is aluminum oxynitride, yittrium oxide, oxygen
Change magnesium, titanium oxide, silica, zinc oxide, described host element purity is the percentage by weight of main element wt and gross weight.
In order to reach above-mentioned requirement, the technical scheme that the present invention uses is the transparent pottery of the high-purity aluminum oxynitride of high transmittance
The preparation method of porcelain, methods described comprise the following steps that.
（1）Nano level nitrogen oxidation aluminium powder doped yttrium oxide, magnesia, titanium oxide, titanium dioxide are chosen by specific proportioning
The nano combined nitrogen oxidation aluminium powder of at least one of silicon, zinc oxide, noresidue binding agent, noresidue surface are put into nano powder
Activating agent, noresidue lubricant, noresidue plasticizer are kneaded.
（2）By step（1）Middle acquisition mixing materials carry out granulation processing, and the grain made is put into injection (mo(u)lding) machine and noted
Penetrate shaping.
（3）By step（2）The middle injection moulding blank that obtains carries out dumping and sintering processes, produces high transmittance High Purity Nitrogen oxygen
Change aluminium crystalline ceramics.
（4）Measuring process（3）The density of middle high transmittance High Purity Nitrogen alumina transparent ceramic, purity, crystallite dimension, bending resistance
Intensity, hardness and straight line transmittance.
The present invention is high transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof, of the invention effective in order to allow, and is needed
Above-mentioned steps are refined, specific thinning parameter is as follows.
Step（1）In, the percentage by weight of aluminum oxynitride is 40% ~ 99% in described nano combined nitrogen oxidation aluminium powder, remaining
Measure as at least one of yittrium oxide, magnesia, titanium oxide, silica, zinc oxide.
Step（1）In, the primary particle size of described nano combined nitrogen oxidation aluminium powder is 1 ~ 100 nanometer.
Step（1）In, the purity of described nano combined nitrogen oxidation aluminium powder is 99.5% ~ 99.999%.
Step（1）In, the percentage by weight of yittrium oxide is 0.1 ~ 10% in the nano combined nitrogen oxidation aluminium powder of selection.
Step（1）In, the percentage by weight of magnesia is 0.1 ~ 10% in the nano combined nitrogen oxidation aluminium powder of selection.
Step（1）In, the percentage by weight of titanium oxide is 0.1 ~ 10% in the nano combined nitrogen oxidation aluminium powder of selection.
Step（1）In, the percentage by weight of silica is 0.1 ~ 20% in the nano combined nitrogen oxidation aluminium powder of selection.
Step（1）In, the percentage by weight of zinc oxide is 0.1 ~ 10% in the nano combined nitrogen oxidation aluminium powder of selection.
Step（1）In, the noresidue binding agent of selection is at least one of high-purity polyvinyl alcohol, high-purity polyvinyl chloride.
Step（1）In, the noresidue surfactant of selection is high-purity octadecanoid acid, high-purity hexadecanoic acid, high-purity 18
At least one of olefin(e) acid.
Step（1）In, the noresidue lubricant of selection is high-purity glycerine, high-purity Tissuemat E, high-purity stearic amide,
At least one of high-purity ethylene base bis-stearamides.
Step（1）In, the noresidue plasticizer of selection is high paraffin refined wax, high-purity dioctyl phthalate, high-purity adjacent benzene
At least one of dioctyl phthalate dicyclohexyl maleate.
Step（1）In, high-purity polyvinyl alcohol purity in the noresidue binding agent of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity polyvinyl chloride purity in the noresidue binding agent of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity octadecanoid acid purity in the noresidue surfactant of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity hexadecanoic acid purity in the noresidue surfactant of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity octadecenic acid purity in the noresidue surfactant of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity glycerine purity in the noresidue lubricant of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity Tissuemat E purity in the noresidue lubricant of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity stearic amide purity in the noresidue lubricant of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity ethylene base bis-stearamides purity in the noresidue lubricant of selection for 99.9% ~
99.999%。
Step（1）In, the high paraffin refined wax purity in the noresidue plasticizer of selection is 99.9% ~ 99.999%.
Step（1）In, high-purity dioctyl phthalate purity in the noresidue plasticizer of selection for 99.9% ~
99.999%。
Step（1）In, high-purity dicyclohexyl phthalate purity in the noresidue plasticizer of selection for 99.9% ~
99.999%。
Step（1）In, the percentage by weight of described nano combined nitrogen oxidation aluminium powder is 80% ~ 90%, and surplus is noresidue
Binding agent, noresidue surfactant, noresidue lubricant, the summation of noresidue plasticizer.
Step（1）In, described mixing time is 2 ~ 48 hours.
Step（1）In, described melting temperature is 120 ~ 170 degree.
Preferably, step（1）In, the primary particle size of described nano combined nitrogen oxidation aluminium powder is 10 ~ 40 nanometers.
Preferably, step（1）In, the purity of described nano combined nitrogen oxidation aluminium powder is 99.99% ~ 99.999%.
Preferably, step（1）In, in the nano combined nitrogen oxidation aluminium powder of selection the percentage by weight of yittrium oxide be 0.1 ~
5%。
Preferably, step（1）In, in the nano combined nitrogen oxidation aluminium powder of selection the percentage by weight of magnesia be 0.1 ~
5%。
Preferably, step（1）In, in the nano combined nitrogen oxidation aluminium powder of selection the percentage by weight of titanium oxide be 0.1 ~
10%。
Preferably, step（1）In, in the nano combined nitrogen oxidation aluminium powder of selection the percentage by weight of silica be 0.1 ~
10%。
Preferably, step（1）In, in the nano combined nitrogen oxidation aluminium powder of selection the percentage by weight of zinc oxide be 0.1 ~
5%。
Preferably, step（1）In, high-purity polyvinyl alcohol purity in the noresidue binding agent of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity polyvinyl chloride purity in the noresidue binding agent of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity octadecanoid acid purity in the noresidue surfactant of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity hexadecanoic acid purity in the noresidue surfactant of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity octadecenic acid purity in the noresidue surfactant of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity glycerine purity in the noresidue lubricant of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity Tissuemat E purity in the noresidue lubricant of selection for 99.99% ~
99.999%。
Preferably, step（1）In, high-purity stearic amide purity in the noresidue lubricant of selection for 99.99% ~
99.999%。
Preferably, step（1）In, the high-purity ethylene base bis-stearamides purity in the noresidue lubricant of selection is
99.99%~99.999%。
Preferably, step（1）In, the high paraffin refined wax purity in the noresidue plasticizer of selection is 99.99% ~ 99.999%.
Preferably, step（1）In, high-purity dioctyl phthalate purity in the noresidue plasticizer of selection is
99.99%~99.999%。
Preferably, step（1）In, high-purity dicyclohexyl phthalate purity in the noresidue plasticizer of selection is
99.99%~99.999%。
Preferably, step（1）In, described mixing time is 4 ~ 24 hours.
Preferably, step（1）In, described melting temperature is 140 ~ 170 degree.
Step（2）In, described prilling process is extruder grain.
Step（2）In, described granulation full-size is 1 ~ 20 millimeter.
Step（2）In, described injection moulding inlet temperature is 120 ~ 170 degree.
Step（2）In, described injection moulding outlet temperature is 100 ~ 140 degree.
Preferably, step（2）In, described granulation full-size is 5 ~ 10 millimeters.
Preferably, step（2）In, described injection moulding inlet temperature is 140 ~ 170 degree.
Preferably, step（2）In, described injection moulding outlet temperature is 120 ~ 130 degree.
Step（3）In, described dumping treatment temperature is 400 ~ 800 degree.
Step（3）In, described dumping processing heating rate is 10 ~ 200 degree/hour.
Step（3）In, described dumping processing rate of temperature fall is 10 ~ 200 degree/hour.
Step（3）In, described dumping processing soaking time is 12 ~ 72 hours.
Step（3）In, described dumping processing atmosphere is air.
Step（3）In, described sintering processes temperature is 1700 ~ 2000 degree.
Step（3）In, described sintering processes soaking time is 1 ~ 10 hour.
Step（3）In, described sintering processes atmosphere is air.
Step（3）In, the described sintering processes temperature rise period is divided into three phases.
Step（3）In, the target temperature of the first stage of the temperature rise period of described sintering processes is 600 ~ 800 degree.
Step（3）In, the heating rate of the first stage of the temperature rise period of described sintering processes for 10 ~ 100 degree/it is small
When.
Step（3）In, the target soaking time of the first stage of the temperature rise period of described sintering processes is small for 0.5 ~ 2
When.
Step（3）In, the target temperature of the second stage of the temperature rise period of described sintering processes is 850 ~ 1700 degree.
Step（3）In, the heating rate of the second stage of the temperature rise period of described sintering processes for 50 ~ 100 degree/it is small
When.
Step（3）In, the target soaking time of the second stage of the temperature rise period of described sintering processes is small for 0.5 ~ 2
When.
Step（3）In, the target temperature of the phase III of the temperature rise period of described sintering processes is 1700 ~ 2000 degree.
Step（3）In, the heating rate of the phase III of the temperature rise period of described sintering processes for 50 ~ 100 degree/it is small
When.
Step（3）In, the target soaking time of the phase III of the temperature rise period of described sintering processes is 1 ~ 10 hour.
Step（3）In, the temperature-fall period of described sintering processes has two stages.
Step（3）In, the target temperature of the first stage of the temperature-fall period of described sintering processes is 800 ~ 1000 degree.
Step（3）In, the rate of temperature fall of the first stage of the temperature-fall period of described sintering processes is 10 ~ 50 degree/hour.
Step（3）In, the target temperature of the second stage of the temperature-fall period of described sintering processes is 20 ~ 80 degree.
Step（3）In, the rate of temperature fall of the second stage of the temperature-fall period of described sintering processes is 10 ~ 80 degree/hour.
Preferably, step（3）In, described dumping treatment temperature is 500 ~ 600 degree.
Preferably, step（3）In, described dumping processing heating rate is 30 ~ 150 degree/hour.
Preferably, step（3）In, described dumping processing rate of temperature fall is 20 ~ 150 degree/hour.
Preferably, step（3）In, described dumping processing soaking time is 24 ~ 60 hours.
Preferably, step（3）In, described sintering processes temperature is 1700 ~ 1850 degree.
Preferably, step（3）In, described sintering processes soaking time is 2 ~ 4 hours.
Preferably, step（3）In, the target temperature of the first stage of the temperature rise period of described sintering processes for 700 ~
800 degree.
Preferably, step（3）In, the heating rate of the first stage of the temperature rise period of described sintering processes is 30 ~ 50
Degree/hour.
Preferably, step（3）In, the target soaking time of the first stage of the temperature rise period of described sintering processes for 1 ~
2 hours.
Preferably, step（3）In, the target temperature of the second stage of the temperature rise period of described sintering processes for 1200 ~
1450 degree.
Preferably, step（3）In, the heating rate of the second stage of the temperature rise period of described sintering processes is 50 ~ 80
Degree/hour.
Preferably, step（3）In, the target soaking time of the second stage of the temperature rise period of described sintering processes for 1 ~
2 hours.
Preferably, step（3）In, the target temperature of the phase III of the temperature rise period of described sintering processes for 1700 ~
1850 degree.
Preferably, step（3）In, the heating rate of the phase III of the temperature rise period of described sintering processes is 50 ~ 80
Degree/hour.
Preferably, step（3）In, the target soaking time of the phase III of the temperature rise period of described sintering processes for 1 ~
4 hours.
Preferably, step（3）In, the target temperature of the first stage of the temperature-fall period of described sintering processes for 900 ~
1000 degree.
Preferably, step（3）In, the rate of temperature fall of the first stage of the temperature-fall period of described sintering processes is 30 ~ 50
Degree/hour.
Preferably, step（3）In, the target temperature of the second stage of the temperature-fall period of described sintering processes is 20 ~ 50
Degree.
Preferably, step（3）In, the rate of temperature fall of the second stage of the temperature-fall period of described sintering processes is 20 ~ 50
Degree/hour.
Step（4）In, described density measuring instrument is Archimedes's drainage density of solid detector.
Step（4）In, described purity detecting instrument is inductively coupled plasma atomic emission spectrometer.
Step（4）In, described crystallite dimension measuring instrument is SEM.
Step（4）In, described bending strength measuring instrument is that three-point bending measures testing machine.
Step（4）In, described hardness measurement instrument is Vickers.
Step（4）In, the measuring instrument of described straight line transmittance is all-wave length light transmittance tester.
Step（4）In, the relative density of described High Purity Nitrogen alumina transparent ceramic is 95 ~ 99.9%.
Step（4）In, the purity of described High Purity Nitrogen alumina transparent ceramic is 99.5 ~ 99.999%.
Step（4）In, the crystallite dimension of described High Purity Nitrogen alumina transparent ceramic is 0.1 ~ 20 micron.
Step（4）In, the bending strength of described High Purity Nitrogen alumina transparent ceramic is 1200 ~ 3000MPa.
Step（4）In, the hardness of described High Purity Nitrogen alumina transparent ceramic is HV2000 ~ 20000.
Step（4）In, the straight line transmittance of described High Purity Nitrogen alumina transparent ceramic is more than 70%.
The present invention is high transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof, is manufactured by present invention process
The following beneficial effect of ceramic structures.
（1）Due to having used superfine nano powder, finished product crystallite dimension is smaller, and intensity is more preferable, and wear extent is small.
（2）Due to the scheme for having used multicomponent to coordinate, make the transmitance of structural member more preferable, shock resistance is more preferably.
（3）Due to having used the dumping sintering process to become more meticulous, allow the density of finished product is higher, and straight line transmittance is more preferable.
Embodiment
The present invention relates to a kind of high transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof, specific implementation step is such as
Under.
（1）It is 2% from yittrium oxide percentage by weight, alumina weight percentage is 1%, and silica weight percentage is
5% aluminum oxynitride composite powder, the host element purity of aluminum oxynitride composite powder is 99.999%, the once grain of aluminum oxynitride composite powder
Footpath is 13.7 nanometers, by composite granule and 99.99% polyvinyl alcohol weight percentage 2%, 99.99% octadecanoid acid weight hundred
Point ratio 3%, 99.99% Tissuemat E percentage by weight 3%, 99.99% paraffin percentage by weight 5% are small in 165 degree of mixings 14
When.
（2）By step（1）It is 9 millimeters that the mixing materials of middle acquisition, which are put into Squeezinggranulator and full-size is granulated at 165 degree,
Particle, then granulated pellet is put into injection (mo(u)lding) machine and is injection moulded, shaping inlet temperature is 170 degree, and outlet temperature is
120 degree, injection moulding blank is obtained, blank for structural product is taken out, and by polishing pouring gate.
（3）By step（2）The blank for structural product of middle acquisition is put into dumping sintering furnace, and heating rate is 40 degree/hour, row
Glue treatment temperature is 600 degree, and the dumping time is 24 hours, and cold with stove, the blank that dumping is finished is put into the first rank in sintering furnace
Section heating rate be 40 degree/hour, and target temperature is 750 degree, and soaking time is 1 hour, second stage heating rate for 60 degree/
Hour, target temperature is 1300 degree, and soaking time is 1 hour, and phase III heating rate is 60 degree/hour, and target temperature is
1750 degree, soaking time is 4 hours, and first stage rate of temperature fall is 40 degree/hour, and target temperature is 1000 degree, second stage
Rate of temperature fall is 30 degree/hour, and target temperature is 30 degree, produces high transmittance High Purity Nitrogen alumina transparent ceramic.
（4）Measuring process（3）The relative density of middle high transmittance High Purity Nitrogen alumina transparent ceramic is 98.83%, and purity is
99.9963%, grain size is 5.9 microns, bending strength 1709MPa, hardness HV18122, straight line transmittance 82%.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, it should all cover within the scope of the present invention.
Claims (10)
1. a kind of high transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof, it is characterised in that comprise the following steps that：
（1）Nano level nitrogen oxidation aluminium powder doped yttrium oxide, magnesia, titanium oxide, silica, oxygen are chosen by specific proportioning
Change the nano combined nitrogen oxidation aluminium powder of at least one of zinc, noresidue binding agent, noresidue surface-active are put into nano powder
Agent, noresidue lubricant, noresidue plasticizer are kneaded；
（2）By step（1）Middle acquisition mixing materials carry out granulation processing, and the grain made is put into injection (mo(u)lding) machine and is injected into
Type；
（3）By step（2）The middle injection moulding blank that obtains carries out dumping and sintering processes, produces the high-purity aluminum oxynitride of high transmittance
Crystalline ceramics；
（4）Measuring process（3）The density of middle high transmittance High Purity Nitrogen alumina transparent ceramic, purity, crystallite dimension, bending resistance are strong
Degree, hardness and straight line transmittance.
2. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（1）In, the percentage by weight of aluminum oxynitride is 40% ~ 99% in described nano combined nitrogen oxidation aluminium powder, and surplus is oxidation
At least one of yttrium, magnesia, titanium oxide, silica, zinc oxide.
3. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（1）In, the purity of described nano combined nitrogen oxidation aluminium powder is 99.5% ~ 99.999%.
4. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（3）In, described sintering processes temperature is 1700 ~ 2000 degree.
5. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（4）In, the relative density of described High Purity Nitrogen alumina transparent ceramic is 95 ~ 99.9%.
6. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（4）In, the purity of described High Purity Nitrogen alumina transparent ceramic is 99.5 ~ 99.999%.
7. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（4）In, the crystallite dimension of described High Purity Nitrogen alumina transparent ceramic is 0.1 ~ 20 micron.
8. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（4）In, the bending strength of described High Purity Nitrogen alumina transparent ceramic is 1200 ~ 3000MPa.
9. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, it is characterised in that：
Step（4）In, the hardness of described High Purity Nitrogen alumina transparent ceramic is HV2000 ~ 20000.
10. high transmittance High Purity Nitrogen alumina transparent ceramic according to claim 1 and preparation method thereof, its feature exists
In：Step（4）In, the straight line transmittance of described High Purity Nitrogen alumina transparent ceramic is more than 70%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272282A (en) * | 2019-06-28 | 2019-09-24 | 上海大学 | The low temperature preparation method of AlON crystalline ceramics |
| CN111018538A (en) * | 2019-11-21 | 2020-04-17 | 天津津航技术物理研究所 | Preparation method of oxynitride medium-wave infrared window material |
| CN111116199A (en) * | 2020-01-18 | 2020-05-08 | 湖南工学院 | Preparation of Gd by vacuum pressureless sintering2Zr2O7Method for making transparent ceramics |
| CN113336567A (en) * | 2021-07-08 | 2021-09-03 | 河南省高新技术实业有限公司 | Preparation method of quartz ceramic membrane support |
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|---|---|---|---|---|
| CN101033140A (en) * | 2007-02-07 | 2007-09-12 | 山东理工大学 | Process for preparing transparent aluminum oxynitride ceramic |
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2017
- 2017-09-19 CN CN201710844569.XA patent/CN107459354A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033140A (en) * | 2007-02-07 | 2007-09-12 | 山东理工大学 | Process for preparing transparent aluminum oxynitride ceramic |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272282A (en) * | 2019-06-28 | 2019-09-24 | 上海大学 | The low temperature preparation method of AlON crystalline ceramics |
| CN110272282B (en) * | 2019-06-28 | 2022-01-07 | 上海大学 | Low-temperature preparation method of AlON transparent ceramic |
| CN111018538A (en) * | 2019-11-21 | 2020-04-17 | 天津津航技术物理研究所 | Preparation method of oxynitride medium-wave infrared window material |
| CN111116199A (en) * | 2020-01-18 | 2020-05-08 | 湖南工学院 | Preparation of Gd by vacuum pressureless sintering2Zr2O7Method for making transparent ceramics |
| CN113336567A (en) * | 2021-07-08 | 2021-09-03 | 河南省高新技术实业有限公司 | Preparation method of quartz ceramic membrane support |
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