CN102030544B - Preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating - Google Patents
Preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating Download PDFInfo
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- CN102030544B CN102030544B CN201010500871A CN201010500871A CN102030544B CN 102030544 B CN102030544 B CN 102030544B CN 201010500871 A CN201010500871 A CN 201010500871A CN 201010500871 A CN201010500871 A CN 201010500871A CN 102030544 B CN102030544 B CN 102030544B
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Abstract
The invention discloses a preparation method of high temperature-resistant, radiation-insulated, heat-conducting and microwave-permeable inorganic coating, which comprises the following steps: preparing sol with ethyl orthosilicate, alcohol, deionized water and hydrochloric acid; synthesizing monox microballoon with the diameter of 0.3-3 micrometers with ethyl orthosilicate, isopropanol, deionized water and ammonia water; growing a titanium oxide shell layer which has the depth from 30-500nm and has high refractivity on the monox microballoon to obtain a stuffing of a nuclear shell structure. The prepared grain with nuclear shell structure is used as the stuffing to be dispersed into the sol so as to be capable of obtaining the compact and even inorganic coating after heat treatment. The added dye with the nuclear shell structure is high in reflectivity to the infrared thermal radiation from 1-10 micrometers, the adding quantity of the stuffing is very small, and the increase of the dielectric constant of the coating is less, so that the preparation method leads the coating to be higher in the thermal reflectivity and not be capable of influencing the microwave permeability, thereby being applied to high-temperature protection at the temperature of 1200 DEG C.
Description
Technical field
The present invention relates to a kind of high temperature resistant separated radiative transfer and pass through the compatible coated material preparation method of microwave; Specifically be meant; Prepare the inorganic coating body material with sol-gel method, and add the functional filler of synthetic nucleocapsid structure, to realize at a distance from radiative transfer and the compatibility of passing through microwave.
Background technology
The basic mode of conducting heat has three kinds of thermal conduction, thermal convection and thermal radiation.Thermal radiation is one of three kinds of basic modes of heat transmission, and along with temperature raises, the radiative transfer proportion increases gradually.Therefore developing high temperature resistant heat insulation material need effectively suppress radiative transfer.Material is launched a large amount of invisible heats under the high temperature, and these invisible heats concentrate on the infrared region of 0.76～10 mu m waveband, and the infrared emanation of shielding 0.76～10 μ m can conduct heat by effective radiation-inhibiting, improves the use temperature and the time of high temperature insulating material.
Stupaliths such as quartz, silicon nitride, as high-temperature structural material can stand high temperature, not be afraid of oxidation, acid-alkali-corrosive-resisting, obtained using widely in fields such as building, automobile and aerospace.But these materials have the section of seeing through at infrared band, so radiation of high temperature is conducted heat very obvious.Stupaliths such as quartz, silicon nitride are at high temperature heated up rapidly, reduce duration of service, and inwardly launch a large amount of invisible heats, therefore inner equipment can lose efficacy.Therefore realize the radiative transfer this type of material at high temperature is under effectively shielded, can prolong material duration of service, protect internal unit.In addition; The specific inductivity of stupaliths such as quartz, silicon nitride is very low; It is good high temperature resistant microwave material; Require the occasion of heat, electrical property at the same time, need effectively not influence its electrical property in the radiation-screening heat transfer, promptly require coating to have the separated radiative transfer performance compatible with passing through microwave.
As yet do not see relevant document at a distance from radiative transfer with the preparation of passing through the compatible coating of microwave for high temperature resistant.
Summary of the invention
A kind of formation of the present invention has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave; Be matrix with silicon oxide or aluminum oxide in this preparation process; The core-shell structure particles that has the anti-infrared thermal radiation performance through interpolation is a filler; Make its ability, do not influence it simultaneously and pass through microwave property with excellent separated radiative transfer.The inorganic coating that makes through the inventive method can pass through the microwave coating material as the high temperature insulating of 1200 ℃ of Working environments.It is a kind of brand-new high temperature resistant heat insulation material that high temperature insulation passes through the microwave coating material, has function heat insulation and that pass through microwave concurrently.Heat insulation mechanism is the infrared emanation under the shielding high temperature, and heat insulation purpose reaches a high temperature.
High temperature resistant at a distance from radiative transfer with pass through the compatible coating of microwave, feed composition mainly contains inorganic sol and core-shell structure particles filler.The present invention selects for use inorganic sol as high temperature resistant filmogen, specifically is selected from silica sol, titanium oxide sol, one or more in alumina sol or the zirconia sol.Described nucleocapsid structure filler particle is spherical, and radius is at 0.3～3 μ m, and the thickness of shell is between 30～500nm.
Above raw material inorganic sol, core-shell structure particles is self-control.
A kind of formation of the present invention has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave, prepares this inorganic coating and realizes through the following step:
Step 1: preparation inorganic sol
(A) in first solvent of 10ml, add the presoma of 5～10g, and stir, obtain precursor solution;
(B) in the deionized water of 10ml, add second solvent of 20～50ml and 5～6 hydrochloric acid (HCl) (volumetric molar concentration is 1mol/L), and stir, obtain the colloidal sol reactant solution;
(C) the colloidal sol reactant solution that step (B) is made is added in the precursor solution that step (A) makes, and low whipping speed is to react 1～12h under the condition of 400～800r/min, and reaction makes inorganic sol after finishing;
Said presoma is own ester of positive silicic acid (TEOS) or aluminum isopropylate (C
9H
21AlO
3).
Said first solvent is ethanol (C
2H
5OH), acetone (C
3H
6O) and ether (C
4H
10O) a kind of in.
Said second solvent is ethanol (C
2H
5OH), acetone (C
3H
6O) and ether (C
4H
10O) a kind of in.
In the present invention, in process for preparation, first solvent will be used identical materials with second solvent.
Step 2: preparation nucleocapsid structure filler
(A) at the ethanol (C of 50ml
2H
5OH) add the inorganic salt of 0.2～2ml and the silica powder (particle diameter 0.3～5 μ m) of 2～10g in, and stir, obtain the filler precursor solution;
Said inorganic salt are tetrabutyl titanate (TBOT) or zirconium oxychloride (ZrOCl
2);
(B) in the deionized water of 10ml, add the ethanol (C of 25～50ml
2H
5OH) and 1～10 percentage concentration be 99% concentrated nitric acid (HNO
3), and stir, obtain the filler reactant solution;
(C) the filler reactant solution that step (B) is made is added in the filler precursor solution that step (A) makes, and is that 25～100 ℃, stirring velocity are to react 2～5h under the condition of 400～800r/min in temperature of reaction, and reaction makes filler solution after finishing;
(D) the filler solution that step (C) is obtained is supersound process 3～10min under the condition of 1000W at ultrasonic power, and is hydro-thermal 2～24h under 140～180 ℃ of conditions in the water heating kettle temperature; Carry out whiz then and obtain filler;
The condition of whiz is: rotating speed 400～800r/min, 70～90 ℃ of drying temperatures, time of drying 2～6h;
(E) filler that step (D) is made to be incubated 2～10h under 300～700 ℃ the temperature, obtains the nucleocapsid structure filler in retort furnace;
Step 3: preparation coated material
The nucleocapsid structure filler that step 2 is made joins in the inorganic sol that step 1 makes, and stirs, and obtains inorganic materials;
The nucleocapsid structure filler that adds 2～10g in the inorganic sol of consumption: 50ml.
Excellent results of the present invention is following:
1, high temperature resistant separated radiative transfer of the present invention and the compatible coated material of microwave thoroughly, its good film-forming property does not ftracture, and does not come off, and preparation technology is simple.
2, the present invention for the single component Ball-type packing, has the effect of very high separated radiative transfer through adding nucleocapsid structure filler granules prepn at a distance from the radiative transfer material, and less to the influence of dielectric properties.
3, coated material of the present invention is a kind of multi-functional coated material, can satisfy the requirement of separated radiative transfer under the high temperature on the one hand, satisfies the requirement of passing through microwave simultaneously.
4, of the present invention high temperature resistant at a distance from radiative transfer with pass through the compatible coating of microwave and can be used for 1200 ℃ high temperature protection.
Description of drawings
Fig. 1 is the embodiment of the invention 1 a nucleocapsid structure filler sem photograph sheet.
Figure 1A is the embodiment of the invention 1 a nucleocapsid structure filler transmission electron microscope picture sheet.
Fig. 2 is that the embodiment of the invention 1 is the surperficial SEM figure of the embodiment of the invention 1100 μ m thick layers.
Fig. 2 A is that the embodiment of the invention 1 is the section SEM figure of the embodiment of the invention 1100 μ m thick layers.
Fig. 3 is that the embodiment of the invention 1 embodiment of the invention 1 coating is at wave number 1000～4000cm
-1The infrared transmittivity collection of illustrative plates.
Fig. 4 be the embodiment of the invention 1 make 100 μ m thick layers specific inductivity with the change of frequency collection of illustrative plates.
Fig. 5 is that the dielectric loss of the embodiment of the invention 1 coating is with the change of frequency collection of illustrative plates.
Embodiment
A kind of formation of the present invention has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave, prepares this inorganic coating and realizes through the following step:
Step 1: preparation inorganic sol
(A) in first solvent of 10ml, add the presoma of 5～10g, and stir, obtain precursor solution;
(B) in the deionized water of 10ml, add second solvent of 20～50ml and 5～6 hydrochloric acid (HCl) (volumetric molar concentration is 1mol/L), and stir, obtain the colloidal sol reactant solution;
(C) the colloidal sol reactant solution that step (B) is made is added in the precursor solution that step (A) makes, and low whipping speed is to react 1～12h under the condition of 400～800r/min, and reaction makes inorganic sol after finishing;
Said presoma is own ester of positive silicic acid (TEOS) or aluminum isopropylate (C
9H
21AlO
3).
Said first solvent is ethanol (C
2H
5OH), acetone (C
3H
6O) and ether (C
4H
10O) a kind of in.
Said second solvent is ethanol (C
2H
5OH), acetone (C
3H
6O) and ether (C
4H
10O) a kind of in.
In the present invention, in process for preparation, first solvent will be used identical materials with second solvent.
Step 2: preparation nucleocapsid structure filler
(A) at the ethanol (C of 50ml
2H
5OH) add the inorganic salt of 0.2～2ml and the silica powder (particle diameter 0.3～5 μ m) of 2～10g in, and stir, obtain the filler precursor solution;
Said inorganic salt are tetrabutyl titanate (TBOT) or zirconium oxychloride (ZrOCl
2);
(B) in the deionized water of 10ml, add the ethanol (C of 25～50ml
2H
5OH) and 1～10 percentage concentration be 99% concentrated nitric acid (HNO
3), and stir, obtain the filler reactant solution;
(C) the filler reactant solution that step (B) is made is added in the filler precursor solution that step (A) makes, and is that 25～100 ℃, stirring velocity are to react 2～5h under the condition of 400～800r/min in temperature of reaction, and reaction makes filler solution after finishing;
(D) the filler solution that step (C) is obtained is supersound process 3～10min under the condition of 1000W at ultrasonic power, and is hydro-thermal 2～24h under 140～180 ℃ of conditions in the water heating kettle temperature; Carry out whiz then and obtain filler;
The condition of whiz is: rotating speed 400～800r/min, 70～90 ℃ of drying temperatures, time of drying 2～6h;
(E) filler that step (D) is made to be incubated 2～10h under 300～700 ℃ the temperature, obtains the nucleocapsid structure filler in retort furnace;
Step 3: preparation coated material
The nucleocapsid structure filler that step 2 is made joins in the inorganic sol that step 1 makes, and stirs, and obtains inorganic materials;
The nucleocapsid structure filler that adds 2～10g in the inorganic sol of consumption: 50ml.
Embodiment 1:
Step 1: preparation inorganic sol
(A) in the ethanol of 10ml, add the own ester of positive silicic acid of 5.7g, and stir, obtain precursor solution;
(B) in the deionized water of 10ml, add 5 of ethanol and the 1mol/L hydrochloric acid solns (HCl) of 20ml, and stir, obtain the colloidal sol reactant solution;
(C) reactant solution that step (B) is made is added in the precursor solution that step (A) makes, and low whipping speed is to react 12h under the condition of 600r/min, and reaction makes inorganic sol after finishing;
Step 2: preparation nucleocapsid structure filler
(A) in the ethanol of 50ml, add the tetrabutyl titanate of 0.4ml and the silica powder (particle diameter 0.3～5 μ m) of 2g, and stir, obtain the filler precursor solution;
(B) concentrated nitric acid (HNO of adding 25ml ethanol and percentage concentration 99% in the deionized water of 10ml
3) 4 droplets, and stir, obtain the filler reactant solution;
(C) the filler reactant solution that step (B) is made is added in the filler precursor solution that step (A) makes, and is that 25 ℃, stirring velocity are to react 2h under the condition of 800r/min in temperature of reaction, and reaction makes filler solution after finishing;
(D) the filler solution that step (C) is obtained is supersound process 5min under the condition of 1000W at ultrasonic power, and is hydro-thermal 20h under 180 ℃ of conditions in the water heating kettle temperature; Carry out whiz then and obtain filler;
The condition of whiz is: rotating speed 400r/min, 90 ℃ of drying temperatures, time of drying 3h;
(E) the filler 700 ℃ of insulation 2h in retort furnace that step (D) made obtain the nucleocapsid structure filler;
The pattern of application scanning Electronic Speculum and transmission electron microscope observing nucleocapsid structure filler, the particle diameter of its nucleocapsid structure filler are at 0.3～5 μ m, and the thickness of shell is between 100～300nm, shown in Fig. 1, Figure 1A.
Step 3: preparation coated material
The nucleocapsid structure filler that step 2 is made joins in the inorganic sol that step 1 makes, and stirs, and obtains inorganic materials;
The nucleocapsid structure filler that adds 8g in the inorganic sol of consumption: 50ml.
Adopt brushing technology on glass substrate, to make the thick film of 80 μ m, use the model of CamScan company to be Apollo300 scanning electron microscopic observation coating pattern, the coating pattern is shown in Fig. 2, Fig. 2 A.Fig. 2 is a surface topography, and Fig. 2 A is the coating cross-section morphology.Can find out inorganic coating surface even compact flawless from the surface scan electromicroscopic photograph, section can find out that coat-thickness is about 80 μ m.
The infrared microwave of coating and dielectric properties such as Fig. 3, Fig. 4 and shown in Figure 5.Can know that by Fig. 3 the coating of adding the nucleocapsid structure filler has tangible shielding effect to thermal radiation, and is little to the influence of dielectric properties simultaneously.Because of SiO
2Fusing point about 1400 ℃, so this coating can be at 1200 ℃ of following life-time service.
The separated radiative transfer performance of coating can characterize with its infrared transmittivity, adopts Nicolet company to produce, and model is NEXUS-470, and the coating infrared transmittivity that intelligent Fourier infrared spectrograph (FTIR) records is as shown in Figure 3.Can know that from Fig. 3 behind the inorganic coating after scribbling 80 μ m on the quartz plate, transmitance is reduced to about 30%.Be that inorganic coating can shield most of infrared emanation, have good separated radiative transfer performance.
The dielectric properties of inorganic coating can change to some extent behind the adding nucleocapsid filler, and adopting U.S.'s Agilent (Agilent) company production model is its dielectric properties variation of vector network analyzer analysis of 8722ES, and test result such as Fig. 4 are shown in 5.Have figure to know, the specific inductivity and the dielectric loss of inorganic coating change not quite behind the adding nucleocapsid structure filler, can not influence its microwave penetrating performance.
Embodiment 2:
Step 1: preparation inorganic sol
(A) in the acetone of 10ml, add the aluminum isopropylate of 10g, and stir, obtain precursor solution;
(B) in the deionized water of 10ml, add the acetone of 50ml and 6 hydrochloric acid (1mol/L), and stir, obtain the colloidal sol reactant solution;
(C) reactant solution that step (B) is made is added in the precursor solution that step (A) makes, and low whipping speed is to react 2h under the condition of 800r/min, and reaction makes inorganic sol after finishing;
Step 2: preparation nucleocapsid structure filler
(A) in the ethanol of 50ml, add the zirconium oxychloride of 2ml and the silica powder (particle diameter 0.3～5 μ m) of 10g, and stir, obtain the filler precursor solution;
(B) concentrated nitric acid (HNO of adding 35ml ethanol and percentage concentration 99% in the deionized water of 10ml
3) 10 droplets, and stir, obtain the filler reactant solution;
(C) the filler reactant solution that step (B) is made is added in the filler precursor solution that step (A) makes, and is that 60 ℃, stirring velocity are to react 3h under the condition of 700r/min in temperature of reaction, and reaction makes filler solution after finishing;
(D) the filler solution that step (C) is obtained is supersound process 8min under the condition of 1000W at ultrasonic power, and is hydro-thermal 10h under 150 ℃ of conditions in the water heating kettle temperature; Carry out whiz then and obtain filler;
The condition of whiz is: rotating speed 800r/min, 70 ℃ of drying temperatures, time of drying 2h;
(E) the filler 300 ℃ of insulation 10h in retort furnace that step (D) made obtain the nucleocapsid structure filler;
The pattern of application scanning Electronic Speculum and transmission electron microscope observing nucleocapsid structure filler, the particle diameter of its nucleocapsid structure is at 0.3～5 μ m, and the thickness of shell is between 300～500nm.
Step 3: preparation coated material
The nucleocapsid structure filler that step 2 is made joins in the inorganic sol that step 1 makes, and stirs, and obtains inorganic materials;
The nucleocapsid structure filler that adds 2～10g in the inorganic sol of consumption: 50ml.
The separated radiative transfer performance of the coating that makes according to embodiment 2 methods can characterize with its infrared transmittivity, and after the coating after scribbling 80 μ m on the quartz plate, transmitance is reduced to about 30%.Be that coating can shield most of infrared emanation, have good separated radiative transfer performance.
The specific inductivity and the dielectric loss of coating change not quite behind the adding nucleocapsid structure filler, can not influence its microwave penetrating performance.
Embodiment 3:
Step 1: preparation inorganic sol
(A) in the ether of 10ml, add the own ester of positive silicic acid of 8g, and stir, obtain precursor solution;
(B) in the deionized water of 10ml, add 5 of ether and the 1mol/L hydrochloric acid solns (HCl) of 30ml, and stir, obtain the colloidal sol reactant solution;
(C) reactant solution that step (B) is made is added in the precursor solution that step (A) makes, and low whipping speed is to react 6h under the condition of 500r/min, and reaction makes inorganic sol after finishing;
Step 2: preparation nucleocapsid structure filler
(A) in the ethanol of 50ml, add the tetrabutyl titanate of 1ml and the silica powder (particle diameter 0.3～5 μ m) of 5g, and stir, obtain the filler precursor solution;
(B) concentrated nitric acid (HNO of adding 35ml ethanol and percentage concentration 99% in the deionized water of 10ml
3) 7 droplets, and stir, obtain the filler reactant solution;
(C) the filler reactant solution that step (B) is made is added in the filler precursor solution that step (A) makes, and is that 60 ℃, stirring velocity are to react 5h under the condition of 500r/min in temperature of reaction, and reaction makes filler solution after finishing;
(D) the filler solution that step (C) is obtained is supersound process 6min under the condition of 1000W at ultrasonic power, and is hydro-thermal 12h under 160 ℃ of conditions in the water heating kettle temperature; Carry out whiz then and obtain filler;
The condition of whiz is: rotating speed 600r/min, 80 ℃ of drying temperatures, time of drying 4h;
(E) the filler 600 ℃ of insulation 6h in retort furnace that step (D) made obtain the nucleocapsid structure filler;
The pattern of application scanning Electronic Speculum and transmission electron microscope observing nucleocapsid structure filler, the particle diameter of its nucleocapsid structure is at 0.3～5 μ m, and the thickness of shell is between 350～500nm.
Step 3: preparation coated material
The nucleocapsid structure filler that step 2 is made joins in the inorganic sol that step 1 makes, and stirs, and obtains inorganic materials;
The nucleocapsid structure filler that adds 2～10g in the inorganic sol of consumption: 50ml
The separated radiative transfer performance of the coating that makes according to embodiment 3 methods can characterize with its infrared transmittivity, and after the coating after scribbling 80 μ m on the quartz plate, transmitance is reduced to about 30%.Be that coating can shield most of infrared emanation, have good separated radiative transfer performance.
The specific inductivity and the dielectric loss of coating change not quite behind the adding nucleocapsid structure filler, can not influence its microwave penetrating performance.
Claims (6)
1. a formation has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave, it is characterized in that preparing this inorganic coating and realizes through the following step:
Step 1: preparation inorganic sol
(A) in first solvent of 10ml, add the presoma of 5～10g, and stir, obtain precursor solution;
(B) in the deionized water of 10ml, adding second solvent of 20～50ml and 5～6 volumetric molar concentration is the hydrochloric acid of 1mol/L, and stirs, and obtains the colloidal sol reactant solution;
(C) the colloidal sol reactant solution that step (B) is made is added in the precursor solution that step (A) makes, and low whipping speed is to react 1～12h under the condition of 400～800r/min, and reaction makes inorganic sol after finishing;
Said presoma is tetraethoxy TEOS or aluminum isopropylate C
9H
21AlO
3;
Said first solvent is ethanol C
2H
5OH, acetone C
3H
6O and ether C
4H
10A kind of among the O;
Said second solvent is ethanol C
2H
5OH, acetone C
3H
6O and ether C
4H
10A kind of among the O;
Step 2: preparation nucleocapsid structure filler
(A) at the ethanol C of 50ml
2H
5Add the inorganic salt of 0.2～2ml and particle diameter 0.3～5 μ m silica powder of 2～10g among the OH, and stir, obtain the filler precursor solution;
Said inorganic salt are tetrabutyl titanate TBOT or zirconium oxychloride ZrOCl
2
(B) in the deionized water of 10ml, add the ethanol C of 25～50ml
2H
5OH and 1～10 percentage concentration is 99% concentrated nitric acid HNO
3, and stir, obtain the filler reactant solution;
(C) the filler reactant solution that step (B) is made is added in the filler precursor solution that step (A) makes, and is that 25～100 ℃, stirring velocity are to react 2～5h under the condition of 400800r/min in temperature of reaction, and reaction makes filler solution after finishing;
(D) the filler solution that step (C) is obtained is supersound process 3～10min under the condition of 1000W at ultrasonic power, and is hydro-thermal 2～24h under 140～180 ℃ of conditions in the water heating kettle temperature; Carry out whiz then and obtain filler;
The condition of whiz is: rotating speed 400～800r/min, 70～90 ℃ of drying temperatures, time of drying 2～6h;
(E) filler that step (D) is made is incubated 2～10h under 300～700 ℃ temperature in retort furnace, obtain the nucleocapsid structure filler;
Step 3: preparation coated material
The nucleocapsid structure filler that step 2 is made joins in the inorganic sol that step 1 makes, and stirs, and obtains inorganic materials;
The nucleocapsid structure filler that adds 2～10g in the inorganic sol of consumption: 50ml.
2. a kind of formation according to claim 1 has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave; It is characterized in that: the particle diameter of the nucleocapsid structure filler that makes in the step 2 is at 0.3～5 μ m, and the thickness of shell is between 30～500nm.
3. a kind of formation according to claim 1 has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave, and it is characterized in that: in the step 1 process for preparation, first solvent will be used identical materials with second solvent.
4. a kind of formation according to claim 1 has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave, it is characterized in that: the inorganic coating surface even compact flawless that makes.
5. a kind of formation according to claim 1 has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave; It is characterized in that: the inorganic coating that 100 μ m are thick can shield 28～60% ir spectra, explains that described inorganic coating has good separated radiative transfer performance.
6. a kind of formation according to claim 1 has high temperature resistant preparation method at a distance from the radiative transfer inorganic coating compatible with passing through microwave; It is characterized in that: the inorganic coating that makes raises at the specific inductivity on the dielectric properties and is lower than 2% and increases in 5% with dielectric loss, can not influence its microwave penetrating performance.
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| CN112811937B (en) * | 2020-12-30 | 2022-07-08 | 哈尔滨工业大学 | Preparation method of high-reflection anti-laser film layer on surface of silicon nitride ceramic substrate |
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