CN115010503A - Use method of sintering aid for transparent oxide ceramic material - Google Patents
Use method of sintering aid for transparent oxide ceramic material Download PDFInfo
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- CN115010503A CN115010503A CN202210660440.4A CN202210660440A CN115010503A CN 115010503 A CN115010503 A CN 115010503A CN 202210660440 A CN202210660440 A CN 202210660440A CN 115010503 A CN115010503 A CN 115010503A
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- 238000005245 sintering Methods 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052574 oxide ceramic Inorganic materials 0.000 title claims description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 101
- 239000000843 powder Substances 0.000 claims abstract description 49
- 238000000498 ball milling Methods 0.000 claims abstract description 20
- 235000015895 biscuits Nutrition 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims abstract 2
- 238000005303 weighing Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000009694 cold isostatic pressing Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 9
- 239000007791 liquid phase Substances 0.000 abstract description 8
- 239000002270 dispersing agent Substances 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 239000011230 binding agent Substances 0.000 abstract 1
- 229920000620 organic polymer Polymers 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 11
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- 238000002834 transmittance Methods 0.000 description 8
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- 229910017109 AlON Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 238000007670 refining Methods 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
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- 229910052596 spinel Inorganic materials 0.000 description 1
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- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 239000011800 void material Substances 0.000 description 1
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Abstract
The invention discloses a method for using an oxide transparent ceramic material sintering aid, which is characterized in that YF is added into oxide powder 3 The form realizes the uniform dispersion of a small amount of sintering aid in oxide powder, is lower than the liquid phase sintering at the traditional sintering temperature of 300 ℃, effectively improves the sintering aid effect through the small amount of sintering aid, and obtains the oxide transparent ceramic. The YF 3 The amount of the sintering aid used as the transparent ceramic oxide is 0.125-0.75at% is prepared by sintering at 1550 ℃ and a lower sintering temperature in a vacuum environment. The YF 3 The sintering aid is added in the ball milling mixing stage and is uniformly mixed with the main component in a planetary ball milling stirring mode; organic polymer materials such as a dispersing agent, a binder and the like do not need to be additionally added, and the formed ceramic biscuit body does not need to be treated in an oxygen atmosphere or other atmospheres.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to YF 3 The preparation of sintering aid in oxide transparent ceramics, in particular to the preparation of yttrium oxide (Y) 2 O 3 ) Application of nano powder in preparing transparent ceramic.
Background
The transparent ceramic material is used as a novel inorganic non-metallic material and is widely applied to optical functional materials and structural materials. For example, YAG transparent ceramic material doped with different rare earth elements can be applied to the fields of laser, scintillation, solid state lighting and the like, MgAl 2 O 4 ，AlON，Al 2 O 3 The transparent ceramic material can be applied to structural materials such as optical protection windows and the like. The sintering aid plays a role in reducing sintering temperature, optimizing microstructure tissues, improving material performance and the like in the preparation process of the ceramic material, and is a magic rod in the preparation process of the ceramic material. The reason why the conventional ceramic powder is difficult to sinter is that the material has high lattice energy, stable crystal structure and high sintering activation energy is required for particle diffusion, becauseThis requires higher temperatures to promote material densification. In order to promote the sintering of such high-energy ionic bond compounds, the addition of a ceramic sintering agent is indispensable. The sintering aid with low melting point is added to generate a low-temperature liquid phase in the sintering process, the liquid phase generates particle bonding and fills air holes under the action of surface tension, and meanwhile, dissolved small crystal grains are gradually deposited on the surfaces of large crystal grains under the action of liquid phase mass transfer by utilizing a dissolution-precipitation mechanism, so that the effect of promoting sintering is achieved. The selection of the effective sintering aid can obviously reduce the sintering temperature of the ceramic, and simultaneously can play roles in refining crystal grains, stabilizing the structure, improving the mechanical property of the material and the like.
In recent years, oxide sintering aids have been mainly used in the field of transparent ceramic production, and for example, patent documents CN107721406A, CN102757237A, CN101851094A and the like use sintering aids to efficiently produce and obtain transparent ceramic samples, and generally, spinel structure ceramics mainly contain CaO, MgO, and AlON ceramics mainly contain SiO 2 Mainly, Y is 2 O 3 Preparation of ceramics with ZrO 2 Mainly comprises the following steps. To reduce the sintering temperature, Y is prepared in a hot-pressing sintering process 2 O 3 LiF is added into the transparent ceramic as a sintering aid. But YF 3 The preparation of the oxide transparent ceramic material for the sintering aid is not reported in documents, and Y is used 2 O 3 Preparation of Y by sintering aid 2 O 3 Transparent ceramics are exemplified. YF 3 The melting point of 1380 ℃ is perfect in matching degree with the crystal lattice of yttrium oxide, and Y can be greatly reduced 2 O 3 Sintering temperature, conventional ZrO 2 Preparation of Y as sintering aid 2 O 3 Transparent ceramics require high temperatures above 1800 c and incorporate a second phase metal element which undoubtedly has a negative effect on the properties of the ceramics. The oxide transparent ceramics can be obtained at the temperature close to the melting point, but the high sintering temperature and the long holding time lead to the rapid growth of the grain size, thereby also reducing the mechanical property of the transparent ceramics.
The invention uses YF 3 The oxide transparent ceramic prepared by the sintering aid has the advantages of small addition amount, good sintering performance and the like, and is expected to be sintered at low temperature of the transparent ceramic if deep research is carried outThe technical field is better applied.
Disclosure of Invention
Aiming at the Y prepared in the prior art 2 O 3 The transparent ceramic of the oxides has low thermal conductivity, high sintering preparation temperature and lattice defect inside the ceramic system, and YF is added in the invention 3 The sintering aid can effectively reduce the sintering temperature, and the transparent oxide ceramic material with high density, high optical transmittance and high thermal conductivity is prepared.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the method comprises two sintering steps: using YF 3 YF preparation as sintering aid 3 Ceramic powder uniformly dispersed in the oxide powder; and sintering by vacuum sintering. The method specifically comprises the following steps:
step 1) weighing: weighing a certain amount of nano oxide (with the particle size range of 0.2-1 μm), wherein the weighing amount is not particularly limited, and the weighed YF 3 0-0.75 at.% of the weighed oxide content, excluding 0; preferably 0.125-0.75 at.%, more preferably 0.5 at.%.
Step 2) mixing materials: and (3) ball milling is carried out for 22-24 hours by using absolute ethyl alcohol as a ball milling medium. And drying the ball-milled slurry in an oven at 80 ℃ for 5-10 hours.
Step 3), powder sieving and forming: grinding the dried slurry, then sieving the ground slurry by a sieve with the particle size of 50-150 mu m, weighing the sieved powder to a certain mass, primarily forming the powder in a steel die, and further compacting the powder after cold isostatic pressing treatment to obtain a ceramic biscuit.
Step 4), vacuum sintering: the obtained oxide ceramic biscuit is placed in< 10 -3 And (3) in a vacuum environment, at the temperature of 1400 ℃ and 1550 ℃, preserving heat for a certain time without annealing, and obtaining the oxide transparent ceramic after polishing.
And 5) in order to further improve the optical transmittance of the oxide transparent ceramic, the transparent ceramic obtained in the step 3 can be subjected to hot isostatic pressing sintering treatment, wherein the sintering temperature is 1500 ℃, the sintering time is 3 hours, and 180 MPa argon is used as an atmosphere.
Preferably, the mass ratio of the ball milling medium anhydrous ethanol to the powder in the step 2) is 2.5:1, and the ball-material ratio is as follows: 3:1, ball milling for 22 hours at the rotating speed of: 235 r/min is the best.
Preferably, the uniaxial pressure for forming the steel mould in the step 3) is 2-5 MPa, the pressure is maintained for 5 s, the cold isostatic pressing is used for improving the density of the biscuit to 200MPa, and the pressure is maintained for 1 min.
Preferably, the optimal sintering temperature of the step 4) is 1450 ℃, and the heat preservation time is 10 hours.
The present invention is directed to the use of YF 3 The nano oxide initial powder is used for preparing the transparent ceramic sintering aid. The method effectively improves the uniformity of grain size distribution in the crystal grains of the oxide transparent ceramic blank to a great extent, is beneficial to the densification of ceramic sintering, and improves the mechanical property of the ceramic material. The method is characterized in that the temperature for preparing the oxide transparent ceramic by adopting the traditional sintering method of vacuum sintering is reduced by about 300 ℃ to obtain the oxide transparent ceramic, the process flow is simple, the operation is easy, and the prepared transparent ceramic has good optical performance.
Drawings
FIG. 1 is the original Y 2 O 3 SEM image of powder, original Y 2 O 3 The powder is mainly of nearly spherical particles, micro-aggregates and nano-scale in size; original Y 2 O 3 The powder had a DSEM of about 71.3 nm; determination of Y by nitrogen adsorption 2 O 3 Specific surface area of powder (SBET), powder specific surface area of 6.35 m 2 /g，Y 2 O 3 Has a density of 5.031 g/cm 3 (ii) a With the original Y 2 O 3 The powder is used as raw material, and YF is quantitatively determined 3 Preparing Y by ceramic preparation processes of sintering aid ball milling, drying, dry pressing/cold isostatic pressing, vacuum presintering and the like 2 O 3 A transparent ceramic;
FIG. 2 shows different YF 3 Sintering the ceramic biscuit with the concentration for 10 hours at 1450 ℃ in a vacuum atmosphere; diffraction peak position and cubic phase Y observed for all ceramics 2 O 3 (PDF # 041-1105); with small amounts of YF 3 As a sintering additive, the YF does not contain a second phase metal element mixed in the transparent ceramic of Y2O3, and does not generate peak position shift caused by lattice defect generated by difference of ionic radius 3 Use of sintering aid to prepare Y 2 O 3 Transparent ceramics are a significant difference from additives used by other researchers;
FIG. 3 is a view of YF 3 Y content of 0.25at.% pre-sintered for 10h at 1450 ℃ under vacuum 2 O 3 Surface SEM image of transparent ceramic; the samples are uniform, the crystal grains do not grow abnormally, the crystal boundary is clear, and no impurity phase (the surface particles are fragments of the ceramic) exists;
FIG. 4 is a view of YF 3 Y with content of 0.50at.% and presintered for 10h at 1450 ℃ under vacuum condition 2 O 3 Surface SEM image of transparent ceramic; pure Y 2 O 3 The surface of the transparent ceramic is provided with clearly visible pores which are a main factor of optical scattering and cause the ceramic to be opaque; it can be seen that YF is the same condition 3 The increase of the content promotes the liquid phase sintering and accelerates Y 2 O 3 Sliding, rearrangement and rotation of the particles while also slightly increasing the grain size, YF 3 The higher the content is, the greater the influence on the grain boundary mobility is;
FIG. 5 is a series of different YF 3 Y with sintering aid content 2 O 3 A picture of a transparent ceramic object, the picture being shown in a small amount of YF 3 Under the effect of combustion assistance, the optical transmittance of the material can be obviously improved;
FIG. 6(a) shows different YF 3 Content Y of 2 O 3 A graph of relative density of the transparent ceramic sample as a function of vacuum sintering temperature; (b) at the same temperature (1450 ℃ C.) Y 2 O 3 The relative density of the transparent ceramic sample was plotted as a function of vacuum sintering time, and in addition, the inset in (b) was Y for different holding times 2 O 3 A physical picture of the transparent ceramic; relative density with YF at the same sintering temperature 3 Increased content while on the same YF 3 At this content, the relative density slightly increases as the sintering temperature increases. The highest relative compactness is YF at all sintering temperatures 3 The content was 0.50at.% of the ceramic sample; YF at 1450 ℃ under different heat preservation times 3 Content Y of 2 O 3 The relative density graph of the transparent ceramic shows that the heat preservation time has little influence on the compactness of the ceramic and is only along with YF 3 The content is increased, and the density is obviously improved; YF with different contents and different heat preservation time 3 Y of (A) is 2 O 3 As can be seen from the ceramic material object diagram, YF 3 Is added to a great extent to increase Y 2 O 3 Transmittance of the ceramic, as illustrated in YF 3 Under the action of (3), the sintering temperature can be greatly reduced to prepare Y 2 O 3 Transparent ceramic samples YF are also described 3 Formation of additives using liquid phase sintering, densification temperature compared to other oxide species Y 2 O 3 The temperature of the transparent ceramic sintering aid is reduced by about 300 ℃; YF 3 As Y 2 O 3 Compared with the existing oxide sintering aid, the sintering aid for the transparent ceramic has an obvious effect;
FIG. 7 shows different YF 3 Content Y of 2 O 3 SEM image of ceramic sample cross section; wherein (a) is 0 at.%; (b) 0.125 at.%; (c) 0.25at%; (d) 0.50 at.%; (e) 0.75at.% Y 2 O 3 A transparent ceramic and (f) an average grain size of 10 hours at 1450 ℃; as can be seen from the figure, the microstructure of the ceramic is similar to the YF 3 Is closely related to the content of YF 3 Increased content void reduction without YF 3 When the auxiliary agent is sintered, the pores in the ceramic sample are more, are mainly distributed at the grain boundary, and are partially communicated holes, so that the ceramic is not compact; these pores are strong scattering centers for light, resulting in the sample being opaque. With YF 3 At Y 2 O 3 The liquid volume for liquid phase sintering is increased due to the increased content in the powder, and Y is increased in the sintering process 2 O 3 The relative displacement between crystal grains and the densification time are prolonged, the sliding speed is accelerated, and the crystal grains grow;
FIG. 8 shows different YF 3 Content miscellaneous ceramic samples (a) UV-Vis-IR transmittance plots; (b) FT-IR transmittance plot; not containing YF 3 The ceramic sample was almost opaque in the visible region, following YF 3 The content is increased, the transmittance is obviously improved, and the highest density is 0.5 percent YF 3 The ceramic sample is 2,4. The transmittances at the wavelength of 6 μm were 76.69, 80.23, and 82.60%, respectively;
FIG. 9 is a series YF 3 Content Y of 2 O 3 Thermal conductivity map of transparent ceramic, different YF 3 Content Y of 2 O 3 The thermal conductivity of the transparent ceramic is changed along with the temperature, the test temperature cannot approach infinity, so the thermal conductivity cannot approach infinity, and Y is increased along with the temperature 2 O 3 The heat conductivity coefficient of the transparent ceramic is reduced; YF 3 Y in an amount of 0.50at% 2 O 3 The thermal conductivity of the transparent ceramic is 14.46W/mK at room temperature and 5.55W/mK at 400 ℃; it is worth noting that with YF 3 Increase in concentration ratio, Y at room temperature 2 O 3 Transparent ceramic YF 3 The thermal conductivity of the ceramic samples with the content of 0, 0.125, 0.25, 0.50 and 0.75at% is respectively 11.25, 12.51, 13.05, 14.42 and 15.56W/m.K; YF 3 Is added to increase Y 2 O 3 Thermal conductivity of transparent ceramics due to YF 3 The higher the content is, the stronger the liquid phase sintering effect is, the pores in the ceramic are eliminated, and the density is increased; meanwhile, the grain size is increased, the area of a grain boundary is reduced, and the heat conductivity of the ceramic is improved.
Detailed Description
The method for using the transparent oxide ceramic sintering aid of the invention is further described with reference to the accompanying drawings and specific examples.
Example one
A method for using an oxide transparent ceramic sintering aid comprises the following specific steps:
(1) weighing: weighing 0.1mol of nano Y 2 O 3 Powder (with particle size of 0.2-1 μm), YF powder 3 The sintering aid is weighed Y 2 O 3 0.50at.% of content;
(2) ball milling: using absolute ethyl alcohol as a powder dispersing agent, and carrying out ball milling on the weighed powder on a star-shaped ball mill for 22 hours to fully and uniformly disperse the weighed powder;
(3) forming: drying the ball-milled dispersed powder, sieving by a 100-mesh sieve to obtain powder, forming the powder by using a hydraulic press under the pressure of 5MPa, and then using cold and the likeFurther obtaining high-compactness Y with uniformly dispersed sintering aids by using a static pressure machine at 200MPa for 1min 2 O 3 A ceramic green body;
(4) and (3) sintering: obtained Y 2 O 3 The ceramic biscuit body is sintered in a vacuum sintering furnace at vacuum degree<10×10 -3 Pa, the sintering temperature is 1450 ℃, and the temperature is kept for 5h to obtain Y 2 O 3 A transparent ceramic.
Example two
A method for using an oxide transparent ceramic sintering aid comprises the following specific steps:
(1) weighing: weighing 0.1mol of nano Y 2 O 3 Powder (the particle size range is 0.2-1 mu m), and the weighed roast chicken additive YF 3 Is the weighed Y 2 O 3 0.25at.% of content;
(2) ball milling: using absolute ethyl alcohol as a powder dispersing agent, and carrying out ball milling on the weighed powder on a star-shaped ball mill for 22 hours to fully and uniformly disperse the weighed powder;
(3) forming: drying the ball-milled dispersed powder, sieving by a 100-mesh sieve to obtain powder, forming the powder by using a hydraulic press under the pressure of 5MPa, and further obtaining the high-compactness Y with uniformly dispersed sintering aid by using a cold isostatic press under the pressure of 200MPa for 1min 2 O 3 A ceramic green body;
(4) and (3) sintering: obtained Y 2 O 3 The ceramic biscuit body is sintered in a vacuum sintering furnace at vacuum degree< 10×10 -3 Pa, the sintering temperature is 1450 ℃, and the temperature is kept for 5h to obtain Y 2 O 3 A transparent ceramic.
EXAMPLE III
A method for using an oxidized transparent ceramic sintering aid comprises the following specific steps:
(1) weighing: weighing 0.5mol of nano MgO powder (the particle size range is 0.2-1 μm), and weighing YF 3 Is 0.25at% of the weighed MgO content;
(2) ball milling: using absolute ethyl alcohol as a powder dispersing agent, and carrying out ball milling on the weighed powder on a star-shaped ball mill for 22 hours to fully and uniformly disperse the weighed powder;
(3) forming: drying the ball-milled dispersed powder, sieving by a 100-mesh sieve to obtain powder, forming the powder by using a hydraulic press under the pressure of 5MPa, and then further obtaining a high-compactness MgO ceramic blank body with uniformly dispersed sintering aids by using a cold isostatic press under the pressure of 200MPa for 1 min;
(4) and (3) sintering: the obtained MgO ceramic biscuit is sintered in a vacuum sintering furnace at vacuum degree< 10×10 -3 Pa, and keeping the sintering temperature of 1450 ℃ for 5h to obtain the MgO transparent ceramic.
Example four
A method for using an oxide transparent ceramic sintering aid comprises the following steps: (1) weighing: weighing 0.5mol of nano CaO powder (the particle size range is 0.2-1 μm), and weighing YF 3 Is 0.50at% of the weighed CaO content;
(2) ball milling: using absolute ethyl alcohol as a powder dispersing agent, and carrying out ball milling on the weighed powder on a star-shaped ball mill for 22 hours to fully and uniformly disperse the weighed powder;
(3) forming: drying the ball-milled dispersed powder, sieving by a 100-mesh sieve to obtain powder, forming the powder by using a hydraulic press under the pressure of 5MPa, and then further obtaining a high-compactness CaO ceramic biscuit with uniformly dispersed sintering aids by using a cold isostatic press under the pressure of 200MPa for 1 min;
(4) and (3) sintering: the obtained CaO ceramic biscuit body is sintered in a vacuum sintering furnace at vacuum degree< 10×10 -3 Pa, and keeping the sintering temperature of 1450 ℃ for 8 h to obtain the CaO transparent ceramic.
EXAMPLE five
The difference between the application method of the oxide transparent ceramic sintering aid and the embodiment is that:
(1) weigh 0.1mol Lu 2 O 3 (the particle size range is 0.2-1 mu m), and the sintering aid is the weighed Lu 2 O 3 0.50at.% of content;
the ball milling and the forming in the step (2) are the same as those in the first embodiment and the third embodiment, and the sintering temperature in the step (4) is 1550 ℃ and is kept for 10 hours.
EXAMPLE six
The use method of the oxide transparent ceramic is different from the embodiment in that:
(1) weigh 0.1mol of Sc 2 O 3 (particle diameter of 0.2 to 1)Mum), the sintering aid is the weighed Sc 2 O 3 0.50at.% of content;
the ball milling in the step (2) and the forming in the step (3) are the same as those in the first embodiment and the third embodiment, and the sintering temperature in the step (4) is 1550 ℃ and the temperature is kept for 10 hours.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. The use method of the sintering aid for the transparent oxide ceramic material is characterized by comprising the following steps: adopting YF 3 Effective as a sintering aid for lower sintering temperatures, the method comprising the steps of:
(1) weighing: weighing oxide and YF 3 ；
(2) Mixing materials: oxide and YF 3 Performing ball milling dispersion in a ball milling medium, and drying the ball milled slurry for later use;
(3) sieving powder and forming: grinding the dried slurry, then sieving, primarily pressing and forming the sieved powder in a die, and further compacting after cold isostatic pressing treatment to obtain a ceramic biscuit;
(4) and (3) sintering: and (4) sintering the ceramic biscuit obtained in the step (3) in a vacuum environment, wherein the obtained oxide transparent ceramic does not need annealing, and double-sided mirror image polished oxide transparent ceramic is obtained after polishing.
2. The method of using the oxide transparent ceramic sintering aid according to claim 1, wherein: YF in step (1) 3 The content is 0.125-0.75 at.% of oxide content.
3. The method of using the oxide transparent ceramic sintering aid of claim 1, wherein: the ball milling medium in the step (2) is absolute ethyl alcohol; the drying temperature is 80 ℃, and the drying time is 5-10 h.
4. The method of using the oxide transparent ceramic sintering aid of claim 1, wherein: the sieving in the step (3) adopts a sieve with the size of 50-150 mu m; the pressure of the primary press forming is 5MPa, and the pressure maintaining time is 5-10 s; the pressure of the cold isostatic pressing is 200MPa, and the pressure maintaining time is 60 s.
5. The method of using the oxide transparent ceramic sintering aid of claim 1, wherein: degree of vacuum during sintering in step (4)< 1×10 -3 (ii) a The sintering temperature is 1400 ℃ and 1550 ℃, and the heat preservation time is 5-10 h.
6. The method of using the oxide transparent ceramic sintering aid of claim 1, wherein: the oxide has high melting point and difficult sintering property, and has higher sintering activity when the particle size is 0.2-1 mu m.
7. The method of using the oxide transparent ceramic sintering aid of claim 2, wherein: the YF 3 The content was 0.50at.% of the oxide content.
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| CN103864409A (en) * | 2014-01-28 | 2014-06-18 | 中国科学院上海光学精密机械研究所 | Preparation method of neodymium-doped yttrium aluminum garnet transparent ceramic |
| US20190276367A1 (en) * | 2018-03-09 | 2019-09-12 | Shin-Etsu Chemical Co., Ltd. | Transparent ceramics, manufacturing method thereof, and magneto-optical device |
| CN110790571A (en) * | 2019-12-10 | 2020-02-14 | 湖南工学院 | Preparation of Gd2Zr2O7Method for making transparent ceramics |
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| CN102020470A (en) * | 2009-09-17 | 2011-04-20 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent yttria ceramics with high optical quality |
| CN103864409A (en) * | 2014-01-28 | 2014-06-18 | 中国科学院上海光学精密机械研究所 | Preparation method of neodymium-doped yttrium aluminum garnet transparent ceramic |
| US20190276367A1 (en) * | 2018-03-09 | 2019-09-12 | Shin-Etsu Chemical Co., Ltd. | Transparent ceramics, manufacturing method thereof, and magneto-optical device |
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