CN113754435B - Y (Y) 2 O 3 Method for preparing MgO infrared transparent ceramic - Google Patents
Y (Y) 2 O 3 Method for preparing MgO infrared transparent ceramic Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000002114 nanocomposite Substances 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000007599 discharging Methods 0.000 claims abstract description 14
- 239000003292 glue Substances 0.000 claims abstract description 14
- 230000005684 electric field Effects 0.000 claims abstract description 11
- 239000011858 nanopowder Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 10
- 238000007731 hot pressing Methods 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 abstract description 9
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000002834 transmittance Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010304 firing Methods 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a Y 2 O 3 A preparation method of MgO infrared transparent ceramics, which belongs to the technical field of transparent ceramic materials; the method comprises the following steps: weigh Y in proportion 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder; placing the nano composite powder into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder; placing the nano composite powder after the glue discharging treatment into a graphite mold, and performing hot-pressing sintering to obtain a complex-phase ceramic blank; the complex phase ceramic body is connected in series in a circuit, electric field intensity is applied to perform flash firing, and high-density Y is obtained after cooling 2 O 3 -MgO ceramic. According to the invention, through hot-press sintering in a graphite die, a large amount of oxygen vacancies are introduced into the complex-phase ceramic blank, so that flash firing can occur in the environment of a lower temperature field and an electric field, and finally, the growth of grain size is inhibited while high density is achieved, the improvement of mechanical properties and the stability of transmittance are facilitated, and the complex-phase ceramic blank can be used as an infrared window material.
Description
Technical Field
The invention relates to a preparation method of an infrared optical window material, in particular to a Y 2 O 3 A method for preparing MgO infrared transparent ceramics, which belongs to the technical field of transparent ceramic materials.
Background
Infrared optical window materials refer to a class of materials used in infrared imaging and guidance techniques to fabricate windows, fairings, etc. These materials have good infrared transparency, a broad transmission band and a certain mechanical strength. In recent years, infrared guided aircrafts are moving towards faster attack speeds and higher hit accuracy, and higher performance requirements, such as higher mechanical properties and lower emissivity, are put on infrared window materials.
In common infrared window materials, Y 2 O 3 Ceramics have high thermal and chemical stability, but low mechanical properties. MgO is introduced as a second phase to suppress Y 2 O 3 Grain growth of the phase, thereby obtaining a phase Y 2 O 3 Y with better mechanical property, thermal shock resistance and good optical permeability of ceramic 2 O 3 -MgO nanocomposite ceramic.
To obtain high transmittance infrared window materials with higher mechanical properties, researchers have proposed a variety of Y' s 2 O 3 -MgO ceramic sintering technology. For example, the invention patent with publication number CN109369183A discloses an infrared transparent ceramic and a preparation method thereof, and the infrared transparent ceramic is prepared from Y 2 O 3 Nanopowder, mgO nanopowder and Gd 2 O 3 A nanocomposite powder comprising nanopowder fired with Gd 2 O 3 The nanometer powder accounts for 0.1-18% of the total molar weight of the nanometer composite powder, and can be sintered by adopting sintering processes such as vacuum sintering, hot-pressing sintering, spark plasma sintering or vacuum hot-pressing sintering, wherein the sintering time is 0.1-15 h, and the sintering temperature is 1100-1850 ℃. The invention uses Gd 2 O 3 The addition of the ceramic material can inhibit the diffusion speed of grain boundary, reduce the growth rate of grains, reduce the grain size of the ceramic material, achieve the purpose of grain refinement and further improve the mechanical properties of the transparent ceramic material.
The invention patent with publication number CN110922169A discloses "a Y 2 O 3 The preparation method of the MgO nano complex phase infrared transparent ceramic adopts Y 2 O 3 The MgO nano multiphase powder is made into a biscuit, and a ceramic blank is obtained by a two-step sintering process in a muffle furnace, wherein the sintering temperature is 1300-1600 ℃, and the heat preservation time is 0.5-100 h; then assisted by hot isostatic pressingSintering at 1200-1500 deg.c for 0.5-5 hr to obtain infrared transparent Y 2 O 3 -MgO nanocomposite ceramic.
The two patents mentioned above relate to Y 2 O 3 The MgO nano complex phase ceramic material and the preparation process have the problems of adding auxiliary agent, expensive sintering equipment, complex and fussy sintering process, high sintering temperature and long heat preservation time, thereby causing Y 2 O 3 The grain size in the MgO complex phase ceramic grows up, ultimately affecting its mechanical properties. Therefore, the sintering process is improved, the sintering time is shortened, and the growth of crystal grains is prevented, so that the high density Y with high transmittance and excellent mechanical property is obtained 2 O 3 MgO nano-composite ceramics remain a challenge to be overcome.
Disclosure of Invention
The purpose of the invention is that: for the existing Y 2 O 3 The sintering process is complex, the sintering temperature is high, the heat preservation time is long, and the sintering auxiliary agent is needed in the MgO nano complex phase ceramic sintering technology, so that the Y is provided 2 O 3 The preparation method of MgO infrared transparent ceramic comprises the steps of hot-pressing and sintering in a graphite die, introducing a large amount of oxygen vacancies into a complex phase ceramic blank, so that flash firing can occur in the environment of a lower temperature field and an electric field, the sintering process can be completed in a period of minutes or even tens of seconds, and finally, the growth of grain size is inhibited while the high density is achieved, thereby being beneficial to the improvement of mechanical properties and the stability of transmittance.
In order to achieve the above purpose, the present invention adopts the following technical scheme: y (Y) 2 O 3 -a method for preparing MgO infrared transparent ceramic, comprising the steps of:
s1: weigh Y in proportion 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder;
s2: placing the nano composite powder obtained in the step S1 into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder;
s3: placing the nano composite powder subjected to the glue discharging treatment in the step S2 into a graphite die, and performing hot-pressing sintering at 900-1200 ℃, 20-40 MPa and 10-30 min to obtain a complex-phase ceramic blank;
s4: the complex phase ceramic blank obtained in the step S3 is connected in series with the two ends of the anode and the cathode of an external power supply by a platinum wire, the electric field intensity of 600-1000V/cm is applied under the condition that the furnace temperature is 1150-1350 ℃, and the current density is controlled to be 20-100 mA/mm after the complex phase ceramic blank is subjected to flash burning 2 And keeping for 10 s-5 min, and cooling in a furnace after finishing to obtain high-density Y 2 O 3 -MgO ceramic.
In the step S1, Y 2 O 3 The volume ratio of MgO nano powder is 1:1.
in the step S4, the current in the circuit is direct current or alternating current.
In the step S4, the cooling method adopts the control cooling in the furnace, and the cooling rate is 2-10 ℃/min.
In the step S4, the cooling method may also use furnace cooling.
The beneficial effects of the invention are as follows:
1) The method of the invention introduces a large amount of oxygen vacancies into the complex phase ceramic blank by hot press sintering in a graphite mold, so that the flash firing can occur in the environment of a lower temperature field and an electric field, thereby completing the sintering process in several minutes or even tens of seconds, finally achieving high density while inhibiting the growth of grain size, and obtaining high density Y with small grain size 2 O 3 -MgO nanocomposite ceramic.
2) The method of the invention is compared with the existing sintering Y 2 O 3 Compared with the MgO ceramic technology, the sintering equipment is simple, the sintering highest temperature is reduced by 300-550 ℃, the sintering time is not more than 5min, and the sintering cost is greatly reduced; and the sintering time is short, the sintering temperature is low, and the growth of the grain size can be avoided, so that the Y with high density and small grain size is obtained 2 O 3 The MgO nano complex phase ceramic is favorable for improving mechanical property and stabilizing transmittance.
Drawings
FIG. 1 is Y prepared in example 1 of the present invention 2 O 3 -scanning electron microscope pictures of MgO nanocomposite ceramic fractures;
FIG. 2 is a table showing the parameter comparison according to an embodiment of the present invention.
Detailed Description
The invention is further illustrated by the following description in conjunction with the accompanying drawings and specific embodiments.
As shown in fig. 1-2, in the embodiment of the present invention, the external Power supply type used for performing flash burning is EA Power Control, and the microscopic photograph scanning device adopts an SEM scanning electron microscope type JSM-7001F.
Example 1: y (Y) 2 O 3 -a method for preparing MgO infrared transparent ceramic, comprising the steps of:
s1: the volume ratio is 1:1 proportion of weighing Y 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder;
s2: placing the nano composite powder obtained in the step S1 into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder;
s3: placing the nano composite powder subjected to the glue discharging treatment in the step S2 into a graphite die, and performing hot-pressing sintering at 1100 ℃, under 30MPa for 20min to obtain a complex-phase ceramic blank;
s4: the complex phase ceramic blank obtained in the step S3 is connected in series with the anode and the cathode of an external power supply by a platinum wire, the electric field intensity of 900V/cm is applied under the condition that the furnace temperature is 1250 ℃, and the current density is controlled to be 60mA/mm after the complex phase ceramic blank is subjected to flash burning 2 And keeping for 1min, cooling in a furnace after finishing, wherein the cooling rate is 10 ℃/min, and obtaining the high-density Y 2 O 3 MgO ceramic with a relative density of 98.8%.
As shown in FIG. 1, Y prepared in example 1 of the present invention 2 O 3 Scanning electron microscope pictures of MgO nano composite ceramic fracture can show that the two phases in the composite material are uniformly distributed, no obvious grain growth phenomenon exists, and the grain sizes are smaller than 1 micron; absence of composite materialObvious defects such as cracks, cavities and the like, which indicate that the Y 2 O 3 The MgO complex phase ceramic has higher density.
Example 2: y (Y) 2 O 3 -a method for preparing MgO infrared transparent ceramic, comprising the steps of:
s1: the volume ratio is 1:1 proportion of weighing Y 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder;
s2: placing the nano composite powder obtained in the step S1 into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder;
s3: placing the nano composite powder subjected to the glue discharging treatment in the step S2 into a graphite die, and performing hot-pressing sintering at the sintering temperature of 1200 ℃, the pressure of 30MPa and the time of 10min to obtain a complex-phase ceramic blank;
s4: the complex phase ceramic blank obtained in the step S3 is connected in series with the anode and the cathode of an external power supply by a platinum wire, the electric field intensity of 1000V/cm is applied under the condition that the furnace temperature is 1150 ℃, and the current density is controlled to be 20mA/mm after the complex phase ceramic blank is subjected to flash burning 2 And keeping for 5min, cooling in a furnace after finishing, wherein the cooling rate is 5 ℃/min, and obtaining the high-density Y 2 O 3 MgO ceramic with a relative density of 97.6%.
Example 3: y (Y) 2 O 3 -a method for preparing MgO infrared transparent ceramic, comprising the steps of:
s1: the volume ratio is 1:1 proportion of weighing Y 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder;
s2: placing the nano composite powder obtained in the step S1 into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder;
s3: placing the nano composite powder subjected to the glue discharging treatment in the step S2 into a graphite die, and performing hot-pressing sintering at 900 ℃, under 40MPa for 30min to obtain a complex-phase ceramic blank;
s4: using the complex phase ceramic blank obtained in the step S3The platinum wire is connected in series with the positive and negative ends of an external power supply, the electric field strength of 600V/cm is applied under the condition that the furnace temperature is 1350 ℃, and the current density is controlled to be 80mA/mm after the flash burning phenomenon of the complex phase ceramic blank occurs 2 And maintaining for 2min, and cooling in the furnace along with the furnace after finishing to obtain high-density Y 2 O 3 MgO ceramic with a relative density of 98.2%.
Example 4: y (Y) 2 O 3 -a method for preparing MgO infrared transparent ceramic, comprising the steps of:
s1: the volume ratio is 1:1 proportion of weighing Y 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder;
s2: placing the nano composite powder obtained in the step S1 into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder;
s3: placing the nano composite powder subjected to the glue discharging treatment in the step S2 into a graphite die, and performing hot-pressing sintering at the sintering temperature of 1200 ℃, the pressure of 20MPa and the time of 20min to obtain a complex-phase ceramic blank;
s4: the complex phase ceramic blank obtained in the step S3 is connected in series with the anode and the cathode of an external power supply by a platinum wire, the electric field intensity of 900V/cm is applied under the condition that the furnace temperature is 1280 ℃, and the current density is controlled to be 100mA/mm after the complex phase ceramic blank is subjected to flash burning 2 And keeping for 10s, cooling in a furnace after the end, wherein the cooling rate is 2 ℃/min, and obtaining the high-density Y 2 O 3 -MgO ceramic with a relative density of 96.4%.
As shown in FIG. 2, from the above embodiment, the method can complete sintering at 1150-1350 ℃, which is 300-550 ℃ lower than the highest sintering temperature of the prior sintering technology, and can complete sintering within 5min, and has the characteristics of low sintering temperature and short sintering time; and Y obtained by this rapid sintering technique 2 O 3 The relative density of MgO complex phase ceramic is higher than 96%, the grain size is not obviously grown, the improvement of mechanical property is facilitated, and the MgO complex phase ceramic can be used as an infrared window material.
The method of the invention is implemented by using stoneHot-press sintering is carried out in an ink mould, and a large number of oxygen vacancies are introduced into a complex phase ceramic blank, so that flash sintering can occur in the environment of a lower temperature field and an electric field, the sintering process can be completed in several minutes or even tens of seconds, and finally, the growth of the grain size is inhibited while the high density is achieved, and the high density Y with small grain size is obtained 2 O 3 -MgO nanocomposite ceramic.
The foregoing is merely illustrative of the present invention and not restrictive, and other modifications and equivalents thereof may occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (1)
1. Y (Y) 2 O 3 -a method for preparing MgO infrared transparent ceramic, comprising the steps of:
s1: the volume ratio is 1:1 proportion of weighing Y 2 O 3 And MgO nano powder are respectively ball-milled, dried and sieved, and uniformly mixed to obtain nano composite powder;
s2: placing the nano composite powder obtained in the step S1 into a muffle furnace for presintering and glue discharging treatment, and removing organic matters in the powder;
s3: placing the nano composite powder subjected to the glue discharging treatment in the step S2 into a graphite die, and performing hot-pressing sintering at 1100 ℃, under 30MPa for 20min to obtain a complex-phase ceramic blank;
s4: the complex phase ceramic blank obtained in the step S3 is connected in series with the anode and the cathode of an external power supply by a platinum wire, the electric field intensity of 900V/cm is applied under the condition that the furnace temperature is 1250 ℃, and the current density is controlled to be 60mA/mm after the complex phase ceramic blank is subjected to flash burning 2 And keeping for 1min, cooling in a furnace after finishing, wherein the cooling rate is 10 ℃/min, and obtaining the high-density Y 2 O 3 MgO ceramic with a relative density of 98.8%.
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