CN115231905B - Preparation method of alumina-based laser attenuation sheet - Google Patents
Preparation method of alumina-based laser attenuation sheet Download PDFInfo
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- CN115231905B CN115231905B CN202210951958.3A CN202210951958A CN115231905B CN 115231905 B CN115231905 B CN 115231905B CN 202210951958 A CN202210951958 A CN 202210951958A CN 115231905 B CN115231905 B CN 115231905B
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Abstract
The invention belongs to the technical field of composite functional materials, and discloses a preparation method of an alumina-based laser attenuation sheet, which comprises the following steps: s1, preparing a ceramic substrate for an attenuation sheet, S2, preparing a quartz substrate for the attenuation sheet, and S3, preparing a laser attenuation sheet. The invention can obtain the excellent laser attenuation sheet with high service life, good attenuation stability, multiple cyclic use and controllable attenuation rate, realizes the aim of rapid and small-batch manufacture of the laser attenuation sheet, solves the key problem that the high laser energy density can cause the damage of the receiver during the laser guidance, and prolongs the service life of the receiver.
Description
Technical Field
The invention belongs to the technical field of composite functional materials, and relates to a preparation method of an alumina-based laser attenuation sheet.
Background
The semi-active laser guidance is widely applied to weapon guidance systems due to the advantages of high guidance positioning precision, strong anti-interference capability, simple structure, high maneuverability and flexibility and the like. However, the high laser energy density causes damage to the receiver, and therefore, it is desirable to design a laser attenuator with excellent performance to reduce the detrimental effects of the high laser energy density.
Disclosure of Invention
Object of the invention
The purpose of the invention is that: aiming at the problem that the laser energy density in the semi-active laser guidance system can cause the damage of a receiving device at present, the preparation method of the alumina-based laser attenuation sheet is provided, the harmful effect of the high laser energy density on a receiver is reduced, and the service life of the receiving device is prolonged.
(II) technical scheme
In order to solve the technical problems, the invention provides a preparation method of an alumina-based laser attenuation sheet, which comprises the following steps:
s1, preparing a ceramic substrate for an attenuation sheet
Preparing ceramic substrate mixed powder: vibrating and mixing alumina powder, lanthanum oxide powder and yttrium oxide powder in a set proportion, and performing circulating high-energy ball milling to obtain mixed powder for a ceramic substrate;
preparing a ceramic substrate: placing the ceramic substrate mixed powder into a mould for compaction, then carrying out hot-pressing sintering, cooling to room temperature at a set speed after heat preservation setting time, taking out the ceramic substrate, and finally grinding to obtain the ceramic substrate with required thickness and surface roughness;
s2, preparing quartz substrate for attenuation sheet
Preparing quartz substrate mixed powder: vibrating and mixing the silicon dioxide powder, the ytterbium oxide powder and the process control agent in a set proportion, and performing circulating high-energy ball milling to obtain mixed powder for the quartz substrate;
preparing a quartz substrate: placing the quartz substrate mixed powder into a mould for compaction, then carrying out hot-pressing sintering, cooling to room temperature at a set speed after heat preservation setting time, taking out the quartz substrate, and finally grinding to obtain the quartz substrate with required thickness and surface roughness;
s3, preparing a laser attenuation sheet
Preparing a bonding layer material: vibrating and mixing the ceramic substrate mixed powder and the quartz substrate mixed powder in a set proportion to obtain a bonding layer material;
preparing a laser attenuation sheet: and adding bonding layer material powder with set thickness between the ceramic substrate and the quartz substrate, placing the bonding layer material powder in a die, then performing spark plasma sintering, cooling to room temperature at a set speed after heat preservation setting time, taking out the bonding layer material powder, then annealing the bonding layer material powder in a heat treatment furnace, and finally performing grinding processing to obtain the laser attenuation sheet with the required thickness and surface roughness.
(III) beneficial effects
According to the preparation method of the alumina-based laser attenuation sheet, the laser attenuation sheet with excellent performance can be obtained, the service life is long, the attenuation stability is good, the laser attenuation sheet can be recycled for multiple times, the attenuation rate is controllable, the aim of rapid and small-batch manufacturing of the laser attenuation sheet is fulfilled, the key problem that the high laser energy density can cause damage to a receiver during laser guidance is solved, and the service life of the receiver is prolonged.
Drawings
FIG. 1 is a flow chart of a method of making an alumina-based laser attenuation sheet of this invention.
Detailed Description
To make the objects, contents and advantages of the present invention more apparent, the following detailed description of the present invention will be given with reference to the accompanying drawings and examples.
FIG. 1 is a flow chart of a method for preparing an alumina-based laser attenuation sheet according to the present invention, as shown in FIG. 1, the method for preparing the alumina-based laser attenuation sheet according to the present invention comprises the steps of:
step one: ceramic substrate for preparing attenuation sheet
Firstly, preparing ceramic substrate mixed powder, and performing hot-pressing sintering molding to obtain the ceramic substrate for the attenuation sheet.
The method comprises the steps of vibrating and mixing alumina powder, lanthanum oxide powder and yttrium oxide powder in a certain proportion, and performing circulating high-energy ball milling to obtain ceramic substrate mixed powder. When the ceramic substrate mixed powder is prepared, the particle size of alumina powder is 50nm, the particle sizes of lanthanum oxide powder and yttrium oxide powder are 30nm, and the mass fraction of the lanthanum oxide powder which is more than 0 percent and less than or equal to 5 percent and the mass fraction of the yttrium oxide powder which is more than 0 percent and less than or equal to 2 percent are satisfied in the mixed powder.
The specific technological parameters of the vibration powder blend are as follows: three-dimensional vibration powder mixing, a 250ml PE plastic tank, a 5mm zirconia grinding ball, a ball-to-material ratio of 3:1, a vibration frequency of 40-60Hz and a vibration time of 1-10h.
The specific technological parameters of the circulating high-energy ball milling process are as follows: planetary ball milling, a 500mL zirconia ball milling tank, 8mm zirconia grinding balls, a ball-to-material ratio of 5:1, a rotating speed of 500rpm, helium atmosphere protection, a ball milling time of 1-8 h, and a ball milling mode of: forward rotation for 15 min-standing for 5 min-reverse rotation for 15 min-standing for 5min, circulating for a period of time, ball milling for 1h, and standing for 1h; and after the circulation high-energy ball milling is completed, the ball milling tank is cooled for 10 hours at room temperature, and then powder taking is carried out in a glove box filled with helium.
After the mixed powder is prepared, the mixed powder is placed in a graphite mold with graphite paper, and is placed on a preformer for prepressing and compacting, and then is sintered by adopting a hot-pressing sintering process. Wherein, the pre-pressing force is 2-10 MPa and the pre-pressing time is 1-15 min; the hot-pressed sintering process is carried out under vacuum degree of less than 10 -3 The sintering is carried out in Pa vacuum atmosphere, the sintering pressure is 30-40 Mpa, and the sintering temperature is 1300-1600 ℃; the sintering process is divided into two steps, namely, the temperature is firstly increased to 40 ℃ below the target sintering temperature at the heating rate of 50 ℃/min, then is increased to the target sintering temperature at the heating rate of 4 ℃/min, the heat preservation time is 30-90 min, and the cooling rate is 50 ℃/min.
And grinding the upper surface and the lower surface of the sintered ceramic substrate to reach the surface roughness Ra 0.4.
Step two: quartz substrate for preparing attenuation sheet
Firstly, preparing quartz substrate mixed powder, and performing hot-pressing sintering molding to obtain the quartz substrate for the attenuation sheet.
And vibrating and mixing the silicon dioxide powder, the ytterbium oxide powder and the process control agent according to a certain proportion, and performing circulating high-energy ball milling to obtain quartz substrate mixed powder. When the quartz substrate mixed powder is prepared, the particle size of silicon dioxide is 50nm, the particle size of ytterbium oxide powder is 30nm, and the mass fraction of the ytterbium oxide powder which is more than 0% and less than or equal to 5% is satisfied in the mixed powder; the process control agent is polyvinyl alcohol, and the mass fraction of the process control agent is less than or equal to 1% and less than 0%.
In the step, specific technological parameters of the vibration powder mixing, the circulating high-energy ball milling and the hot-pressing sintering process are consistent with those of the step one.
And grinding the upper surface and the lower surface of the sintered quartz substrate to reach the surface roughness Ra 0.4.
Step three: preparation of laser attenuation sheet
Firstly, preparing bonding layer material mixed powder, clamping the bonding layer material mixed powder between a ceramic substrate and a quartz substrate with a certain thickness, and sintering and forming by using spark plasma to obtain the laser attenuation sheet.
When the bonding layer material mixed powder is prepared, the mass ratio of the ceramic substrate mixed powder to the quartz substrate mixed powder is 5:1-1:5, and the concrete process of vibration powder mixing is consistent with the step one.
Spark plasma sintering at vacuum degree less than 10 -3 The sintering is carried out in the vacuum atmosphere of Pa, the sintering pressure is 30Mpa, and the sintering temperature is 1200-1500 ℃; the sintering process is divided into two steps, namely, the temperature is firstly increased to 100 ℃ below the target sintering temperature at the heating rate of 100 ℃/min, then is increased to the target sintering temperature at the heating rate of 20 ℃/min, the heat preservation time is 30-90 min, and the cooling rate is 50 ℃/min.
Annealing the sintered laser attenuation sheet, heating to 1550 ℃ in a vacuum muffle furnace at a speed of 80 ℃/min, and keeping for 40min; then cooling to 900 ℃ at a speed of 5 ℃/min, turning off the power supply of the heating furnace, and naturally cooling to room temperature along with the furnace.
In the annealed laser attenuation sheet, the ceramic substrate is ground to 0.1-2 mm, the quartz substrate is ground to 0.5-3 mm, and the surface roughness of the laser attenuation sheet reaches Ra0.2.
The ceramic substrate and the quartz substrate with excellent performances can be obtained by proper hot pressing sintering pressure, sintering temperature and heat preservation time.
The laser attenuation sheet with excellent performance can be obtained by proper spark plasma sintering pressure, sintering temperature and heat preservation time.
The following is a specific description of two preferred embodiments:
example 1:
step one: preparing a ceramic substrate for an attenuation sheet: alumina powder with the particle size of 50nm, lanthanum oxide powder with the mass fraction of 30nm which is 1% and yttrium oxide powder with the mass fraction of 30nm which is 2% are placed in a 250ml PE plastic tank, 5mm zirconium oxide grinding balls are added according to the ball-to-material ratio of 3:1, the vibration frequency is 50Hz, and the vibration time is 2 hours. Then removing 5mm balls from the powder after vibration mixing, placing the powder in a zirconia ball milling tank, adding 8mm zirconia balls according to a ball-to-material ratio of 5:1, and introducing helium for 1min after closing a cover; placing the pot in a ball mill, wherein the ball milling mode is planetary ball milling, the rotation speed is 500rpm, the ball milling time is 2 hours, the specific process comprises forward rotation for 15 minutes, standing for 5 minutes, reverse rotation for 15 minutes, standing for 5 minutes, and taking the process as a cycle of one hour, and stopping cooling the ball milling pot for 1 hour after the ball milling accumulated time is 1 hour; after the ball milling is completed, the ball milling tank is cooled for 10 hours, and then powder is taken in a glove box filled with helium.
Placing the prepared mixed powder into a graphite mold with graphite paper and a diameter of 52mm, and compacting on a preformer, wherein the preforming pressure is 6MPa, and the preforming time is 5min; sintering the pre-pressed graphite mould filled with the mixed powder in a hot-pressing sintering furnace, wherein the sintering is carried out under the pressure of 10 -3 The vacuum atmosphere of (2) is carried out by firstly heating the hot-press sintering furnace to 1460 ℃ at a heating rate of 50 ℃/min, then heating to 1500 ℃ at a heating rate of 4 ℃/min, then preserving heat for 50min under the pressure of 40MPa, and finally cooling to 40 ℃ at a cooling rate of 50 ℃/min, and taking out the sample. And grinding the sample until the surface roughness is Ra0.4, thereby preparing the ceramic substrate for the attenuation sheet.
Step two: preparing a quartz substrate for an attenuation sheet: silica powder with the particle size of 50nm, ytterbium oxide powder with the mass fraction of 30nm which is 1% and polyvinyl alcohol with the mass fraction of 1% are placed in a 250ml PE plastic tank, 5mm zirconium oxide grinding balls are added according to the ball-to-material ratio of 3:1, the vibration frequency is 50Hz, and the vibration time is 2 hours. Then removing 5mm balls from the powder after vibration mixing, placing the powder in a zirconia ball milling tank, adding 8mm zirconia balls according to a ball-to-material ratio of 5:1, and introducing helium for 1min after closing a cover; placing the pot in a ball mill, wherein the ball milling mode is planetary ball milling, the rotation speed is 500rpm, the ball milling time is 3 hours, the specific process comprises forward rotation for 15 minutes, standing for 5 minutes, reverse rotation for 15 minutes, standing for 5 minutes, and taking the process as a cycle of one hour, and stopping cooling the ball milling pot for 1 hour after the ball milling accumulated time is 1 hour; after the ball milling is completed, the ball milling tank is cooled for 10 hours, and then powder is taken in a glove box filled with helium.
Placing the prepared mixed powder into a graphite mold with graphite paper and a diameter of 52mm, and compacting on a preformer, wherein the preforming pressure is 8MPa, and the preforming time is 5min; sintering the pre-pressed graphite mould filled with the mixed powder in a hot-pressing sintering furnace, wherein the sintering is carried out under the pressure of 10 -3 The vacuum atmosphere of (2) is carried out by firstly heating the hot-press sintering furnace to 1360 ℃ at a heating rate of 50 ℃/min, then heating to 1400 ℃ at a heating rate of 4 ℃/min, then preserving heat for 60min under the pressure of 40MPa, and finally cooling to 40 ℃ at a cooling rate of 50 ℃/min, and taking out the sample. And then grinding the sample until the surface roughness is Ra0.4, thereby preparing the quartz substrate for the attenuation sheet.
Step three: preparing a laser attenuation sheet: and (3) adding the ceramic substrate mixed powder prepared in the step (I) and the quartz substrate mixed powder prepared in the step (II) into a 250ml PE plastic tank according to the mass ratio of 1:1, and adding a 5mm zirconia grinding ball according to the ball-to-material ratio of 3:1, wherein the vibration frequency is 50Hz, and the vibration time is 2h. Then placing the mixture in a graphite mold with graphite paper and a diameter of 52mm, placing the mixture in a discharge plasma sintering furnace for sintering, wherein the sintering is carried out under a pressure of 10 -3 The vacuum atmosphere of (2) is carried out by firstly raising the temperature of the discharge plasma sintering furnace to 1400 ℃ at the heating rate of 100 ℃/min, then raising the temperature to 1500 ℃ at the heating rate of 20 ℃/min, then preserving the heat under the pressure of 30MPa for 60min, and finally taking out the sample when the sample is cooled to 40 ℃ at the cooling rate of 50 ℃/min. Then heating to 1550 ℃ in a vacuum muffle furnace at a speed of 80 ℃/min, and keeping for 40min; then cooling to 900 ℃ at a speed of 5 ℃/min, turning off the power supply of the heating furnace, and naturally cooling to room temperature along with the furnace. And finally grinding the sample, wherein the ceramic substrate is required to be ground to 1mm, the quartz substrate in the laser attenuation sheet is required to be ground to 2mm, and the roughness of the two surfaces is Ra0.4, so that the laser attenuation sheet is prepared.
Example 2:
step one: preparing a ceramic substrate for an attenuation sheet: alumina powder with the particle size of 50nm, lanthanum oxide powder with the mass fraction of 30nm which is 1% and yttrium oxide powder with the mass fraction of 30nm which is 1% are placed in a 250ml PE plastic tank, 5mm zirconium oxide grinding balls are added according to the ball-to-material ratio of 3:1, the vibration frequency is 50Hz, and the vibration time is 2 hours. Then removing 5mm balls from the powder after vibration mixing, placing the powder in a zirconia ball milling tank, adding 8mm zirconia balls according to a ball-to-material ratio of 5:1, and introducing helium for 1min after closing a cover; placing the pot in a ball mill, wherein the ball milling mode is planetary ball milling, the rotation speed is 500rpm, the ball milling time is 2 hours, the specific process comprises forward rotation for 15 minutes, standing for 5 minutes, reverse rotation for 15 minutes, standing for 5 minutes, and taking the process as a cycle of one hour, and stopping cooling the ball milling pot for 1 hour after the ball milling accumulated time is 1 hour; after the ball milling is completed, the ball milling tank is cooled for 10 hours, and then powder is taken in a glove box filled with helium.
Placing the prepared mixed powder into a graphite mold with graphite paper and a diameter of 52mm, and compacting on a preformer, wherein the preforming pressure is 6MPa, and the preforming time is 5min; sintering the pre-pressed graphite mould filled with the mixed powder in a hot-pressing sintering furnace, wherein the sintering is carried out under the pressure of 10 -3 The vacuum atmosphere of (2) is carried out by firstly heating the hot-press sintering furnace to 1460 ℃ at a heating rate of 50 ℃/min, then heating to 1500 ℃ at a heating rate of 4 ℃/min, then preserving heat for 50min under the pressure of 40MPa, and finally cooling to 40 ℃ at a cooling rate of 50 ℃/min, and taking out the sample. And grinding the sample until the surface roughness is Ra0.4, thereby preparing the ceramic substrate for the attenuation sheet.
Step two: preparing a quartz substrate for an attenuation sheet: silica powder with the particle size of 50nm, ytterbium oxide powder with the mass fraction of 30nm which is 1% and polyvinyl alcohol with the mass fraction of 1% are placed in a 250ml PE plastic tank, 5mm zirconium oxide grinding balls are added according to the ball-to-material ratio of 3:1, the vibration frequency is 50Hz, and the vibration time is 2 hours. Then removing 5mm balls from the powder after vibration mixing, placing the powder in a zirconia ball milling tank, adding 8mm zirconia balls according to a ball-to-material ratio of 5:1, and introducing helium for 1min after closing a cover; placing the pot in a ball mill, wherein the ball milling mode is planetary ball milling, the rotation speed is 500rpm, the ball milling time is 3 hours, the specific process comprises forward rotation for 15 minutes, standing for 5 minutes, reverse rotation for 15 minutes, standing for 5 minutes, and taking the process as a cycle of one hour, and stopping cooling the ball milling pot for 1 hour after the ball milling accumulated time is 1 hour; after the ball milling is completed, the ball milling tank is cooled for 10 hours, and then powder is taken in a glove box filled with helium.
Placing the prepared mixed powder into a graphite mold with graphite paper and a diameter of 52mm, and compacting on a preformer, wherein the preforming pressure is 8MPa, and the preforming time is 5min; sintering the pre-pressed graphite mould filled with the mixed powder in a hot-pressing sintering furnace, wherein the sintering is carried out under the pressure of 10 -3 The vacuum atmosphere of (2) is carried out by firstly heating the hot-press sintering furnace to 1360 ℃ at a heating rate of 50 ℃/min, then heating to 1400 ℃ at a heating rate of 4 ℃/min, then preserving heat for 60min under the pressure of 40MPa, and finally cooling to 40 ℃ at a cooling rate of 50 ℃/min, and taking out the sample. And then grinding the sample until the surface roughness is Ra0.4, thereby preparing the quartz substrate for the attenuation sheet.
Step three: preparing a laser attenuation sheet: and (3) adding the ceramic substrate mixed powder prepared in the step (A) and the quartz substrate mixed powder prepared in the step (B) into a 250ml PE plastic tank according to the mass ratio of 1:2, and adding a 5mm zirconia grinding ball according to the ball-to-material ratio of 3:1, wherein the vibration frequency is 60Hz, and the vibration time is 2h. Then placing the mixture in a graphite mold with graphite paper and a diameter of 52mm, placing the mixture in a discharge plasma sintering furnace for sintering, wherein the sintering is carried out under a pressure of 10 -3 The vacuum atmosphere of (2) is carried out by firstly raising the temperature of the discharge plasma sintering furnace to 1400 ℃ at the heating rate of 100 ℃/min, then raising the temperature to 1500 ℃ at the heating rate of 20 ℃/min, then preserving the heat for 80min under the pressure of 30MPa, and finally taking out the sample when the sample is cooled to 40 ℃ at the cooling rate of 50 ℃/min. Then heating to 1550 ℃ in a vacuum muffle furnace at a speed of 80 ℃/min, and keeping for 40min; then cooling to 900 ℃ at a speed of 5 ℃/min, turning off the power supply of the heating furnace, and naturally cooling to room temperature along with the furnace. And finally grinding the sample, wherein the ceramic substrate is required to be ground to 3mm, the quartz substrate in the laser attenuation sheet is required to be ground to 1mm, and the roughness of the two surfaces is Ra0.4, so that the laser attenuation sheet is prepared.
Table 1 shows attenuation rate data processed by the preparation method of the alumina-based laser attenuation sheet according to table 1, which can illustrate that the processing technology of the invention has the advantages of long service life, good attenuation stability, multiple times of recycling, controllable attenuation rate, realization of the goal of rapid small-batch manufacturing of the laser attenuation sheet, solving the key problem that the high laser energy density can cause the damage of a receiver during laser guidance, and prolonging the service life of the receiver.
TABLE 1 decay Rate data for example 1 and example 2 before and after the inventive treatment
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and variations could be made by those skilled in the art without departing from the technical principles of the present invention, and such modifications and variations should also be regarded as being within the scope of the invention.
Claims (1)
1. The preparation method of the alumina-based laser attenuation sheet is characterized by comprising the following steps of:
s1, preparing a ceramic substrate for an attenuation sheet
Preparing ceramic substrate mixed powder: vibrating and mixing alumina powder, lanthanum oxide powder and yttrium oxide powder in a set proportion, and performing circulating high-energy ball milling to obtain mixed powder for a ceramic substrate;
preparing a ceramic substrate: placing the ceramic substrate mixed powder into a mould for compaction, then carrying out hot-pressing sintering, cooling to room temperature at a set speed after heat preservation setting time, taking out the ceramic substrate, and finally grinding to obtain the ceramic substrate with required thickness and surface roughness;
s2, preparing quartz substrate for attenuation sheet
Preparing quartz substrate mixed powder: vibrating and mixing the silicon dioxide powder, the ytterbium oxide powder and the process control agent in a set proportion, and performing circulating high-energy ball milling to obtain mixed powder for the quartz substrate;
preparing a quartz substrate: placing the quartz substrate mixed powder into a mould for compaction, then carrying out hot-pressing sintering, cooling to room temperature at a set speed after heat preservation setting time, taking out the quartz substrate, and finally grinding to obtain the quartz substrate with required thickness and surface roughness;
s3, preparing a laser attenuation sheet
Preparing a bonding layer material: vibrating and mixing the ceramic substrate mixed powder and the quartz substrate mixed powder in a set proportion to obtain a bonding layer material;
preparing a laser attenuation sheet: adding bonding layer material powder with set thickness between the ceramic substrate and the quartz substrate, placing the bonding layer material powder in a die, then performing spark plasma sintering, cooling to room temperature at a set speed after heat preservation setting time, taking out the bonding layer material powder, then annealing the bonding layer material powder in a heat treatment furnace, and finally performing grinding processing to obtain the laser attenuation sheet with required thickness and surface roughness;
in the step S1, in the ceramic substrate mixed powder, the particle size of alumina powder is 50nm, the particle sizes of lanthanum oxide powder and yttrium oxide powder are 30nm, and the mass fraction of lanthanum oxide powder is more than 0 percent and less than or equal to 5 percent, and the mass fraction of yttrium oxide powder is more than 0 percent and less than or equal to 2 percent;
in the step S2, in the quartz substrate mixed powder, the particle size of the silicon dioxide powder is 50nm, the particle size of the ytterbium oxide powder is 30nm, and the mass fraction of the ytterbium oxide powder which is more than 0 percent is less than or equal to 5 percent; the process control agent is polyvinyl alcohol, which satisfies the mass fraction of 0% < process control agent less than or equal to 1%;
in the step S3, in the bonding layer material powder, the mass ratio of the ceramic substrate mixed powder to the quartz substrate mixed powder is 5:1-1:5;
in the steps S1-S3, the technological parameters of vibration powder mixing are as follows: three-dimensional vibration powder mixing, a 250ml PE plastic tank, a 5mm zirconia grinding ball, a ball-to-material ratio of 3:1, a vibration frequency of 40-60Hz and a vibration time of 1-10h;
in the steps S1-S2, the technological parameters of the circulating high-energy ball milling process are as follows: planetary ball milling, a 500mL zirconia ball milling tank, 8mm zirconia grinding balls, a ball-to-material ratio of 5:1, a rotating speed of 500rpm, helium atmosphere protection, a ball milling time of 1-8 h, and a ball milling mode of: forward rotation for 15 min-standing for 5 min-reverse rotation for 15 min-standing for 5min, circulating for a period of time, ball milling for 1h, and standing for 1h; after the circulation high-energy ball milling is completed, cooling the ball milling tank at room temperature for 10 hours, and taking powder in a glove box filled with helium;
in the steps S1-S2, the hot-press sintering process is as follows:
placing the mixed powder into a graphite mould with graphite paper, placing the graphite mould on a prepressing machine for prepressing and compacting, and sintering by adopting a hot-pressing sintering process; when in prepressing, the prepressing force is 2-10 MPa, and the prepressing time is 1-15 min; the hot-pressed sintering process is carried out under vacuum degree of less than 10 -3 The sintering is carried out in Pa vacuum atmosphere, the sintering pressure is 30-40 Mpa, and the sintering temperature is 1300-1600 ℃; the sintering process is divided into two steps, namely, the temperature is firstly increased to 40 ℃ below the target sintering temperature at the heating rate of 50 ℃/min, then is increased to the target sintering temperature at the heating rate of 4 ℃/min, the heat preservation time is 30-90 min, and then the cooling rate is 50 ℃/min;
in the step S3, spark plasma sintering is performed under vacuum degree of less than 10 -3 The sintering is carried out in the vacuum atmosphere of Pa, the sintering pressure is 30Mpa, and the sintering temperature is 1200-1500 ℃; the spark plasma sintering process is divided into two steps, namely, the temperature is firstly increased to 100 ℃ below the target sintering temperature at the heating rate of 100 ℃/min, then the temperature is increased to the target sintering temperature at the heating rate of 20 ℃/min, the heat preservation time is 30-90 min, and then the cooling rate is 50 ℃/min;
in the step S3, the annealing process of the laser attenuation sheet includes: heating to 1550 ℃ in a vacuum muffle furnace at a speed of 80 ℃/min, and keeping for 40min; then cooling to 900 ℃ at a speed of 5 ℃/min, turning off the power supply of the heating furnace, and naturally cooling to room temperature along with the furnace;
in the step S1, the upper surface and the lower surface of the ceramic substrate are ground to have the surface roughness Ra0.4 after sintering; in the step S2, the upper surface and the lower surface of the quartz substrate are ground to have the surface roughness Ra0.4 after sintering; in the step S3, the ceramic substrate in the annealed laser attenuation sheet is ground to 0.1-2 mm, the quartz substrate is ground to 0.5-3 mm, and the surface roughness of the laser attenuation sheet reaches Ra0.2.
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