CN116813366A - Hamburger type ceramic-crystal composite substrate and preparation method thereof - Google Patents
Hamburger type ceramic-crystal composite substrate and preparation method thereof Download PDFInfo
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- CN116813366A CN116813366A CN202310615919.0A CN202310615919A CN116813366A CN 116813366 A CN116813366 A CN 116813366A CN 202310615919 A CN202310615919 A CN 202310615919A CN 116813366 A CN116813366 A CN 116813366A
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- 239000002131 composite material Substances 0.000 title claims abstract description 81
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- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 106
- 239000002159 nanocrystal Substances 0.000 claims abstract description 80
- 239000000463 material Substances 0.000 claims abstract description 57
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- 239000010439 graphite Substances 0.000 claims description 11
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- 239000000203 mixture Substances 0.000 claims description 10
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- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 5
- 229910002601 GaN Inorganic materials 0.000 claims description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 5
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
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- 239000012535 impurity Substances 0.000 claims description 5
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- 229910044991 metal oxide Inorganic materials 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 5
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 229910052594 sapphire Inorganic materials 0.000 claims description 5
- 239000010980 sapphire Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
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- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
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- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 6
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/02—Constructional details
- H01S3/025—Constructional details of solid state lasers, e.g. housings or mountings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
- C03C3/112—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
- C03C3/115—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron
- C03C3/118—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron containing aluminium
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
- H01S3/06—Construction or shape of active medium
- H01S3/0602—Crystal lasers or glass lasers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
- H01S3/1685—Ceramics
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- Materials Engineering (AREA)
- Optics & Photonics (AREA)
- Ceramic Engineering (AREA)
- Plasma & Fusion (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a hamburger type ceramic-crystal composite substrate and a preparation method thereof, wherein the hamburger type ceramic-crystal composite substrate comprises a ceramic sheet and at least two nanocrystalline sheets, wherein the ceramic sheet and the at least two nanocrystalline sheets are sintered at low temperature, and the two side surfaces of the ceramic sheet are preprocessed to form bonding surfaces; preprocessing one side surface or two side surfaces of the nanocrystal sheet to form a bonding surface; the nano crystal plates are bonded on two sides of the ceramic plate in a layered and symmetrical mode to form a hamburger structure, and bonding material layers are coated between bonding surfaces; the preparation method comprises the steps of preparation of ceramic sheets and crystal sheets, cleaning, drying, acid washing, plasma cleaning and activating, bonding interface material coating, pressing, heat treatment and the like. The ceramic-crystal composite substrate can realize bonding at a temperature lower than the melting point of crystals, has low requirement on the flatness of bonding surfaces, can form micron-sized transition interfaces between ceramics and crystals, and has the advantages of no interface defect, large bonding force and good optical uniformity.
Description
Technical Field
The invention relates to the field of semiconductor material processing, in particular to a hamburger type ceramic-crystal composite substrate and a preparation method thereof.
Background
With the continuous development and popularization of laser crystal technology, more and more fields begin to use laser crystals widely, and more fields are used: nd is YAG, yb is YAG, etc.; wherein Yb-YAG refers to trivalent ytterbium ion (Yb 3+ ) A laser crystal producing a near infrared laser of 1.03. 1.03 um is formed by doping a matrix of Yttrium Aluminum Garnet (YAG), which is the same matrix as Nd-YAG, but has a different growth process due to the different doping. The Yb doped YAG has high quantum efficiency (91%), simple crystal spectrum, no excitation state absorption and up-conversion, no fluorescence concentration quenching, high doping concentration, long fluorescence lifetime (0.91 ms) and effective coupling with the pumping wavelength of the diode; in addition, the YAG matrix has the most excellent physical and chemical characteristics and comprehensive performance, so that the Nd-YAG crystal is one of the most attractive solid laser media and is regarded as one main direction for developing high-efficiency and high-power solid lasers.
Compared with the existing common monocrystalline laser material, the transparent laser ceramic has the advantages of simple preparation, low cost, large size, high concentration doping, good thermal shock resistance, mass production and the like, and is a very potential solid laser material. In particular, the preparation of the ceramic-ceramic and ceramic-single crystal composite structure laser gain material by bonding and other processes greatly enriches the realizable forms of the laser gain medium.
The bonding technology is a technology that the contact surfaces of homogeneous or heterogeneous crystals with clean surfaces and atomic-level roughness are directly attached to form a whole under certain conditions, and wafers are bonded together through chemical bonds. Compared with the gluing technology, the technology has great superiority, and by the mode, the bonding material with smooth and even interface and optical transparency can be obtained, and has important significance for solving the heat dissipation, light guide and other innovative application of crystals. However, bonding is a complex process technology, and since optical crystals mostly have a very high melting point, the conventional bonding process needs to perform high-temperature heat treatment close to the melting point, and simultaneously apply a certain pressure on the contact surface to make surface atoms of two crystals mutually diffuse and fuse, so that a stable chemical bond is finally formed. However, the thermal bonding method has the defects that the gas in the bonding surface is difficult to diffuse out and the pressure is uneven, cracks are easily generated on the bonding surface, the lattice structure is easily changed at an excessively high temperature, and the like.
Disclosure of Invention
The invention aims to: the invention aims to provide a hamburger type ceramic-crystal composite substrate and a preparation method thereof, which can improve the processing quality of ceramic plates and crystal plates.
The technical scheme is as follows: the invention relates to a hamburger type ceramic-crystal composite substrate, which comprises:
the ceramic plate is formed by low-temperature sintering, and bonding surfaces are formed by pretreatment of two side surfaces of the ceramic plate;
at least two nanocrystal pieces, wherein one side surface or two side surfaces of the nanocrystal pieces are pretreated to form a bonding surface;
wherein, the nano crystal sheet is bonded on two sides of the ceramic sheet in a layered and symmetrical way to form a hamburger structure, and bonding material layers are coated between bonding surfaces.
Preferably, the bonding material layer is formed by proportioning the following powder in percentage by mass:
SiO 2 the mass percentage is 20-60%;
Al 2 O 3 the mass percentage is 30-45%;
Na 2 o accounts for 0-10 percent by mass;
B 2 O 3 the mass percentage is 0-10%;
K 2 o accounts for 0-10 percent by mass;
ZnO accounts for 0-8 percent by mass;
MgO is 0-8% by mass;
the mass percentage of CuO is 0-5%;
CaF 2 the mass percentage is 0-3%.
Preferably, the doping concentrations of the nanocrystal sheet and the ceramic sheet are distributed in a stepwise manner, and the doping concentrations are continuously increased along the pumping direction.
Preferably, the surface finish of the bonding surface is not less than 10/5, the flatness is less than lambda/4, and the roughness is not more than 0.5 nm.
Preferably, the low-temperature sintered ceramic sheet is one of oxide ceramic, fluoride ceramic and metal oxide ceramic.
Preferably, the nano crystal sheet is one of sapphire, monocrystalline silicon, gallium arsenide, gallium nitride and silicon carbide.
The invention also discloses a preparation method of the hamburger type ceramic-crystal composite substrate, which comprises the following steps:
step S 1 : preparing a ceramic sheet and a nanocrystal sheet sintered at low temperature, polishing the bonding surface, and wiping the bonding surface by using a cleaning wiper to remove organic impurities;
step S 2 : ultrasonic cleaning the ceramic sheet and the nano crystal sheet after wiping treatment to remove the residual grinding particles, dissolved residues and organic matters on the bonding surface; placing the ceramic sheet and the nano crystal sheet in an oven, and drying under the conditions that the drying temperature is 45-190 ℃ and the drying time is 2.5-6 h;
step S 3 : soaking the dried ceramic sheet and the dried nano crystal sheet in a mixed acid solution with the volume ratio of sulfuric acid and phosphoric acid=1:5.5 and the concentration of 12-21% for 15-45 min, and removing oxides on the surfaces of the ceramic sheet and the nano crystal sheet; then, the mixture is washed by deionized water and soaked in cyclohexane solution to isolate air;
step S 4 : placing the ceramic sheet and the nano crystal sheet together with cyclohexane solution in a plasma cleaning machine, adding an ethylenediamine tetraacetic acid activator with the concentration of 5mmol/l, and cleaning and activating the bonding surfaces of the ceramic sheet and the nano crystal sheet;
step S 5 : the bonding interface material is diluted and then is uniformly coated or sprayed on the ceramicBonding material layers are formed on bonding surfaces of the sheets and the nano crystal sheets, the bonding surfaces of the ceramic sheets and the nano crystal sheets are tightly adhered and are pressed and fixed by a graphite clamp, and the clamping pressure is 12-32 Kg/cm 2 The dwell time is 1-4 h, and a composite substrate sample is prepared;
step S 6 : placing the composite substrate sample with pressure maintaining in a vacuum hot pressing furnace for heat treatment;
step S 7 : and taking out the composite substrate sample subjected to heat treatment from the vacuum hot pressing furnace, and opening the graphite clamp to obtain the composite substrate formed by bonding the ceramic sheet and the nano crystal sheet.
Preferably, step S 6 The heat treatment specifically comprises the following steps:
step S 61 : heating the composite substrate sample to an annealing temperature of 70-600 ℃ at a heating rate of 5-7 ℃/min, and an annealing time of 20-70 h;
step S 62 : the material sample after the annealing treatment is cooled to room temperature at a cooling rate of 3-5 ℃/min.
Preferably, step S 5 The medium bonding interface diluting material specifically comprises the following steps:
step S 51 : weighing and mixing the powder in a proportion uniformly, feeding the powder mixture into a crystal slurry thickener for thickening, and enabling the crystal slurry after thickening to flow into a centrifugal machine through a circular pipe in a gravity flow mode for solid-liquid separation to obtain a bonding interface material with high purity;
step S 52 : diluting the bonding interface material with any one of absolute ethyl alcohol, distilled water or deionized water, and diluting at stirring speed of 130-350 r/min for 15-25 min.
Preferably, step S 1 Or step S 2 The cleaning solution is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts low-temperature bonding to prepare the hamburger type ceramic-crystal composite substrate, and the melting point of the nano material can be reduced along with the reduction of the particle size based on the scale effect by selecting nano crystals, thereby greatly reducing the temperature and pressure requirements in the bonding process; the ceramic material is sintered at low temperature, is suitable for high current and high temperature resistance, and is suitable for manufacturing a multilayer circuit substrate, and has the advantages of short production period, small volume, light weight, low cost, energy conservation and environmental protection;
2. the ceramic-crystal composite substrate adopts the bonding interface material, realizes bonding between crystal atoms at a temperature far lower than the melting point of crystals, has mild heating conditions and low energy consumption, has low requirements on the flatness of bonding surfaces, can form a layer of micron-sized transition interface between ceramics and crystals and between crystals and has no interface defect at the bonding interface, and has large bonding force and good optical uniformity;
3. the ceramic-crystal composite substrate adopts the multilayer gradient doped crystals, so that the ceramic-crystal composite substrate is fully pumped, the doping concentration is continuously increased along the pumping direction, the composite substrate has uniform pumping power density and thermal field distribution, the energy storage density and total energy storage of the center of the composite substrate are improved, the internal temperature tends to be gentle along with the increase of the degree of compounding, and the uniform distribution of heat in the material is facilitated;
4. the composite substrate with the gradient doping structure can be applied to an advanced solid laser, and the laser performance with high power, high efficiency and excellent beam quality is obtained.
Drawings
FIG. 1 is a schematic illustration of a process flow for preparing an embodiment of a ceramic-crystal composite substrate of the present invention;
FIG. 2 is a schematic illustration of a process flow for preparing a ceramic-crystal composite substrate according to another embodiment of the present invention.
Reference numerals:
1. a ceramic sheet; 2. a crystal plate; 3. a bonding material layer; 4. a graphite jig; 5. a pressurized load; 6. a composite substrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1-2 of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which are obtained by a person skilled in the art based on the described embodiments of the invention, fall within the scope of protection of the invention.
Example 1:
as shown in fig. 1-2, the "hamburger" ceramic-crystal composite substrate of the invention comprises a ceramic sheet 1 and two nanocrystalline sheets 2, wherein the ceramic sheet 1 is sintered at low temperature, the ceramic sheet 1 is one of oxide ceramic, fluoride ceramic and metal oxide ceramic, and the nanocrystalline sheet 2 is one of sapphire, monocrystalline silicon, gallium arsenide, gallium nitride and silicon carbide. The two side surfaces of the ceramic sheet 1 are pretreated to form bonding surfaces, and one side surface or two side surfaces of the nanocrystal sheet 2 are pretreated to form bonding surfaces, so that the process requirements of the bonding surfaces are as follows: the surface finish is not less than 10/5, the flatness is less than lambda/4, and the roughness is not more than 0.5 and nm. The nanocrystal pieces 2 are bonded in a layered and symmetrical manner on two sides of the ceramic piece 1 to form a hamburger structure, bonding material layers 3 are coated between bonding surfaces, and the bonding material layers 3 are formed by mixing the following powder according to mass percent: siO (SiO) 2 Is 20% by mass of Al 2 O 3 45 mass percent of Na 2 O is 5% by mass, B 2 O 3 Is 5% by mass, K 2 The mass percent of O is 5%, the mass percent of ZnO is 6%, the mass percent of MgO is 6%, the mass percent of CuO is 5%, and the mass percent of CaF is 6% 2 The mass percentage of (2) is 3%.
According to the ceramic-crystal composite substrate, the nano crystal is selected, and the melting point of the nano material is reduced along with the reduction of the particle size due to the scale effect, so that the temperature and the pressure in the bonding process are greatly reduced; the low-temperature sintered ceramic is selected, is suitable for high current and high temperature resistance, and is suitable for manufacturing a multilayer circuit substrate; by using a bonding interface material, bonding between crystal atoms is achieved at a temperature well below the melting point of the crystal. The composite substrate attaching structure is a hamburg type structure, one or more crystal sheets are respectively arranged above and below the ceramic sheet, the doping concentrations of the nano crystal sheet 2 and the ceramic sheet 1 are distributed in a stepwise manner, so that the ceramic-crystal composite substrate is fully pumped, and as the ceramic and the crystal are of a multilayer combined structure, a person skilled in the art can obtain a pumping direction according to the combined analysis of the ceramic and the crystal, the doping concentration is continuously increased along the pumping direction, so that the ceramic-crystal composite substrate has uniform pumping power density and thermal field distribution, the energy storage density and total energy storage of the center of the ceramic-crystal composite substrate are improved, the internal temperature tends to be gentle along with the increase of the degree of recombination, and the uniform distribution of heat in the material is facilitated; the ceramic-crystal composite substrate with the gradient doping structure can be applied to an advanced solid laser to obtain laser performance with high power, high efficiency and excellent beam quality.
Example 2:
as shown in fig. 1-2, the "hamburger" ceramic-crystal composite substrate of the invention comprises a ceramic sheet 1 and at least two nano crystal sheets 2, wherein the ceramic sheet 1 is sintered at a low temperature, the low temperature is one of oxide ceramic, fluoride ceramic and metal oxide ceramic, and the nano crystal sheet 2 is one of sapphire, monocrystalline silicon, gallium arsenide, gallium nitride and silicon carbide. The two side surfaces of the ceramic sheet 1 are pretreated to form bonding surfaces, and one side surface or two side surfaces of the nanocrystal sheet 2 are pretreated to form bonding surfaces, so that the process requirements of the bonding surfaces are as follows: the surface finish is not less than 10/5, the flatness is less than lambda/4, and the roughness is not more than 0.5 and nm. The nanocrystal pieces 2 are bonded in a layered and symmetrical manner on two sides of the ceramic piece 1 to form a hamburger structure, bonding material layers 3 are coated between bonding surfaces, and the bonding material layers 3 are formed by mixing the following powder according to mass percent: siO (SiO) 2 Is 60% by mass of Al 2 O 3 Is 30% by mass, B 2 O 3 Is 5% by mass, 3% by mass of MgO, caF 2 The mass percentage of (2%).
According to the ceramic-crystal composite substrate, the nano crystal is selected, and the melting point of the nano material is reduced along with the reduction of the particle size due to the scale effect, so that the temperature and the pressure in the bonding process are greatly reduced; the low-temperature sintered ceramic is selected, is suitable for high current and high temperature resistance, and is suitable for manufacturing a multilayer circuit substrate; bonding between crystal atoms is achieved at a temperature well below the melting point of the crystal by using a bonding interface material; the composite substrate attaching structure is a hamburg type structure, one or more crystal sheets are respectively arranged above and below the ceramic sheet, the doping concentrations of the nano crystal sheet 2 and the ceramic sheet 1 are distributed in a stepwise manner, so that the ceramic-crystal composite substrate is fully pumped, and as the ceramic and the crystal are of a multilayer combined structure, a person skilled in the art can obtain a pumping direction according to the combined analysis of the ceramic and the crystal, the doping concentration is continuously increased along the pumping direction, so that the ceramic-crystal composite substrate has uniform pumping power density and thermal field distribution, the energy storage density and total energy storage of the center of the ceramic-crystal composite substrate are improved, the internal temperature tends to be gentle along with the increase of the degree of recombination, and the uniform distribution of heat in the material is facilitated; the ceramic-crystal composite substrate with the gradient doping structure can be applied to an advanced solid laser to obtain laser performance with high power, high efficiency and excellent beam quality.
Example 3:
as shown in fig. 1-2, the "hamburger" ceramic-crystal composite substrate of the invention comprises a ceramic sheet 1 and at least two nano crystal sheets 2, wherein the ceramic sheet 1 is sintered at a low temperature, the low temperature is one of oxide ceramic, fluoride ceramic and metal oxide ceramic, and the nano crystal sheet 2 is one of sapphire, monocrystalline silicon, gallium arsenide, gallium nitride and silicon carbide. The two side surfaces of the ceramic sheet 1 are pretreated to form bonding surfaces, and one side surface or two side surfaces of the nanocrystal sheet 2 are pretreated to form bonding surfaces, so that the process requirements of the bonding surfaces are as follows: the surface finish is not less than 10/5, the flatness is less than lambda/4, and the roughness is not more than 0.5 and nm. The nanocrystal pieces 2 are bonded in a layered and symmetrical manner on two sides of the ceramic piece 1 to form a hamburger structure, bonding material layers 3 are coated between bonding surfaces, and the bonding material layers 3 are formed by mixing the following powder according to mass percent: siO (SiO) 2 40 mass percent of Al 2 O 3 37 mass percent of Na 2 7% of O, 8% of ZnO, 5% of CuO and CaF 2 The mass percentage of (2) is 3%.
According to the ceramic-crystal composite substrate, the nano crystal is selected, and the melting point of the nano material is reduced along with the reduction of the particle size due to the scale effect, so that the temperature and the pressure in the bonding process are greatly reduced; the low-temperature sintered ceramic is selected, is suitable for high current and high temperature resistance, and is suitable for manufacturing a multilayer circuit substrate; bonding between crystal atoms is achieved at a temperature well below the melting point of the crystal by using a bonding interface material; the composite substrate attaching structure is a hamburg type structure, one or more crystal sheets are respectively arranged above and below the ceramic sheet, the doping concentrations of the nano crystal sheet 2 and the ceramic sheet 1 are distributed in a stepwise manner, so that the ceramic-crystal composite substrate is fully pumped, and as the ceramic and the crystal are of a multilayer combined structure, a person skilled in the art can obtain a pumping direction according to the combined analysis of the ceramic and the crystal, the doping concentration is continuously increased along the pumping direction, so that the ceramic-crystal composite substrate has uniform pumping power density and thermal field distribution, the energy storage density and total energy storage of the center of the ceramic-crystal composite substrate are improved, the internal temperature tends to be gentle along with the increase of the degree of recombination, and the uniform distribution of heat in the material is facilitated; the ceramic-crystal composite substrate with the gradient doping structure can be applied to an advanced solid laser to obtain laser performance with high power, high efficiency and excellent beam quality.
Example 4:
the invention also discloses a preparation method of the hamburger type ceramic-crystal composite substrate, which comprises the following steps:
(1) Preparing a ceramic sheet 1 and a nanocrystal sheet 2 sintered at low temperature, polishing the bonding surface, and wiping the bonding surface by using a cleaning wiper to remove organic impurities; wherein the cleaning agent is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone;
(2) Ultrasonic cleaning is carried out on the ceramic sheet 1 and the nano crystal sheet 2 after the wiping treatment to remove the residual abrasive particles, dissolved residues and organic matters on the bonding surface; placing the ceramic sheet 1 and the nano crystal sheet 2 in an oven, and drying under the conditions that the drying temperature is 45 ℃ and the drying time is 6 h; wherein the cleaning solution is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone;
(3) Placing the dried ceramic sheet 1 and the dried nanocrystal sheet 2 in a volume ratio of: sulfuric acid, namely, immersing the ceramic plate 1 and the nano crystal plate 2 in a mixed acid solution with the concentration of 12% and composed of phosphoric acid=1:5.5 for 45 min to remove oxides on the surfaces of the ceramic plate and the nano crystal plate; then, the mixture is washed by deionized water and soaked in cyclohexane solution to isolate air;
(4) Placing the ceramic sheet 1 and the nano crystal sheet 2 together with cyclohexane solution in a plasma cleaning machine, adding an ethylenediamine tetraacetic acid activator with the concentration of 5mmol/l, and cleaning and activating the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2;
(5) The bonding interface material is diluted and then is evenly coated or sprayed on the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2 to form a bonding material layer 3, the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2 are closely adhered and are pressed and fixed by using a graphite clamp 4, and the clamping pressure is 12 Kg/cm 2 The dwell time was 4 h, producing a composite substrate sample; the bonding interface diluting material specifically comprises the following steps:
(1) weighing and mixing the powder in a proportion uniformly, feeding the powder mixture into a crystal slurry thickener for thickening, and enabling the crystal slurry after thickening to flow into a centrifugal machine through a circular pipe in a gravity flow mode for solid-liquid separation to obtain a bonding interface material with high purity;
(2) diluting the bonding interface material by taking a proper amount of any one of absolute ethyl alcohol, distilled water or deionized water, and diluting for 25 min at the stirring speed of 130 r/min;
(6) Placing the composite substrate sample with pressure maintaining in a vacuum hot pressing furnace for heat treatment; the method specifically comprises the following steps:
(1) heating the composite substrate sample at a heating rate of 5 ℃/min to an annealing temperature of 70 ℃ and an annealing time of 70 h;
(2) cooling the material sample subjected to annealing treatment to room temperature at a cooling rate of 3 ℃/min;
(7) And taking out the composite substrate sample subjected to heat treatment from the vacuum hot pressing furnace, and opening the graphite clamp 4 to obtain the composite substrate 6 formed by bonding the ceramic sheet 1 and the nanocrystal sheet 2.
Example 5:
the invention also discloses a preparation method of the hamburger type ceramic-crystal composite substrate, which comprises the following steps:
(1) Preparing a ceramic sheet 1 and a nanocrystal sheet 2 sintered at low temperature, polishing the bonding surface, and wiping the bonding surface by using a cleaning wiper to remove organic impurities; wherein the cleaning agent is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone;
(2) Ultrasonic cleaning is carried out on the ceramic sheet 1 and the nano crystal sheet 2 after the wiping treatment to remove the residual abrasive particles, dissolved residues and organic matters on the bonding surface; placing the ceramic sheet 1 and the nano crystal sheet 2 in an oven, and drying under the conditions that the drying temperature is 190 ℃ and the drying time is 2.5 h; wherein the cleaning solution is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone;
(3) Placing the dried ceramic sheet 1 and the dried nanocrystal sheet 2 in a volume ratio of: sulfuric acid, namely, a mixed acid solution with the concentration of 21% and composed of phosphoric acid=1:5.5 is soaked for 15 min, and oxides on the surfaces of the ceramic sheet 1 and the nano crystal sheet 2 are removed; then, the mixture is washed by deionized water and soaked in cyclohexane solution to isolate air;
(4) Placing the ceramic sheet 1 and the nano crystal sheet 2 together with cyclohexane solution in a plasma cleaning machine, adding an ethylenediamine tetraacetic acid activator with the concentration of 5mmol/l, and cleaning and activating the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2;
(5) The bonding interface material is diluted and then is evenly coated or sprayed on the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2 to form a bonding material layer 3, the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2 are closely adhered and are pressed and fixed by using a graphite clamp 4, and the clamping pressure is 32 Kg/cm 2 The dwell time was 1 h, a composite substrate sample was prepared; the bonding interface diluting material specifically comprises the following steps:
(1) weighing and mixing the powder in a proportion uniformly, feeding the powder mixture into a crystal slurry thickener for thickening, and enabling the crystal slurry after thickening to flow into a centrifugal machine through a circular pipe in a gravity flow mode for solid-liquid separation to obtain a bonding interface material with high purity;
(2) diluting the bonding interface material by taking a proper amount of any one of absolute ethyl alcohol, distilled water or deionized water, and diluting for 15 min at a stirring speed of 350 r/min;
(6) Placing the composite substrate sample with pressure maintaining in a vacuum hot pressing furnace for heat treatment; the method specifically comprises the following steps:
(1) heating the composite substrate sample at a heating rate of 7 ℃/min to an annealing temperature of 600 ℃ and an annealing time of 20 h;
(2) cooling the material sample subjected to annealing treatment to room temperature at a cooling rate of 5 ℃/min;
(7) And taking out the composite substrate sample subjected to heat treatment from the vacuum hot pressing furnace, and opening the graphite clamp 4 to obtain the composite substrate 6 formed by bonding the ceramic sheet 1 and the nanocrystal sheet 2.
Example 6:
the invention also discloses a preparation method of the hamburger type ceramic-crystal composite substrate, which comprises the following steps:
(1) Preparing a ceramic sheet 1 and a nanocrystal sheet 2 sintered at low temperature, polishing the bonding surface, and wiping the bonding surface by using a cleaning wiper to remove organic impurities; wherein the cleaning agent is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone;
(2) Ultrasonic cleaning is carried out on the ceramic sheet 1 and the nano crystal sheet 2 after the wiping treatment to remove the residual abrasive particles, dissolved residues and organic matters on the bonding surface; placing the ceramic sheet 1 and the nano crystal sheet 2 in an oven, and drying under the conditions that the drying temperature is 115 ℃ and the drying time is 4 h; wherein the cleaning solution is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone;
(3) Placing the dried ceramic sheet 1 and the dried nanocrystal sheet 2 in a volume ratio of: sulfuric acid, namely soaking the ceramic chip 1 and the nano crystal chip 2 in a mixed acid solution with the concentration of 16% and consisting of phosphoric acid=1:5.5 for 30 min to remove oxides on the surfaces of the ceramic chip 1 and the nano crystal chip 2; then, the mixture is washed by deionized water and soaked in cyclohexane solution to isolate air;
(4) Placing the ceramic sheet 1 and the nano crystal sheet 2 together with cyclohexane solution in a plasma cleaning machine, adding an ethylenediamine tetraacetic acid activator with the concentration of 5mmol/l, and cleaning and activating the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2;
(5) The bonding interface material is diluted and then is evenly coated or sprayed on the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2 to form a bonding material layer 3, the bonding surfaces of the ceramic sheet 1 and the nano crystal sheet 2 are closely adhered and are pressed and fixed by using a graphite clamp 4, and the clamping pressure is 22 Kg/cm 2 The dwell time was 2.5 h, producing a composite substrate sample; the bonding interface diluting material specifically comprises the following steps:
(1) weighing and mixing the powder in a proportion uniformly, feeding the powder mixture into a crystal slurry thickener for thickening, and enabling the crystal slurry after thickening to flow into a centrifugal machine through a circular pipe in a gravity flow mode for solid-liquid separation to obtain a bonding interface material with high purity;
(2) diluting the bonding interface material by taking a proper amount of any one of absolute ethyl alcohol, distilled water or deionized water, and diluting for 20 min at a stirring speed of 240 r/min;
(6) Placing the composite substrate sample with pressure maintaining in a vacuum hot pressing furnace for heat treatment; the method specifically comprises the following steps:
(1) heating the composite substrate sample at a heating rate of 6 ℃/min to an annealing temperature of 335 ℃ and an annealing time of 45 h;
(2) cooling the material sample subjected to annealing treatment to room temperature at a cooling rate of 4 ℃/min;
(7) And taking out the composite substrate sample subjected to heat treatment from the vacuum hot pressing furnace, and opening the graphite clamp 4 to obtain the composite substrate 6 formed by bonding the ceramic sheet 1 and the nanocrystal sheet 2.
In the above embodiments 4-6, the high-temperature heat treatment process of the composite substrate sample adopts the double-heat source vacuum hot-pressing furnace, the vacuum hot-pressing furnace adopts the hot air and the radiant heat source to heat in a matching way, and applies the pressure load in the high-temperature heat treatment process, so as to accelerate the diffusion and migration of atoms and molecules of the bonding surface between the ceramic sheet 1 and the nanocrystal sheet 2, and the bonding material layer 3 can fill the tiny gaps formed by the processing defects of the bonding surface, thereby improving the quality of the composite substrate.
The foregoing is a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A "hamburger" ceramic-crystal composite substrate comprising:
a ceramic sheet (1) sintered at a low temperature, wherein bonding surfaces are formed by preprocessing two side surfaces of the ceramic sheet (1);
at least two nanocrystal pieces (2), wherein one side surface or two side surfaces of the nanocrystal pieces (2) are pretreated to form a bonding surface;
wherein the nanocrystal pieces (2) are symmetrically bonded in layers at two sides of the ceramic piece (1) to form a hamburger structure, and bonding material layers (3) are coated between bonding surfaces.
2. The hamburger type ceramic-crystal composite substrate according to claim 1, wherein the bonding material layer (3) is formed by the following powder ingredients according to mass percent:
SiO 2 the mass percentage is 20-60%;
Al 2 O 3 the mass percentage is 30-45%;
Na 2 o accounts for 0-10 percent by mass;
B 2 O 3 the mass percentage is 0-10%;
K 2 o accounts for 0-10 percent by mass;
ZnO accounts for 0-8 percent by mass;
MgO is 0-8% by mass;
the mass percentage of CuO is 0-5%;
CaF 2 the mass percentage is 0-3%.
3. The ceramic-crystal composite substrate according to claim 1, characterized in that the doping concentration of the nanocrystalline chips (2) and ceramic chips (1) is stepwise distributed and the doping concentration continuously increases in the pumping direction.
4. The ceramic-crystal composite substrate of claim 1, wherein the bonding surface has a surface finish of not less than 10/5, a flatness of less than λ/4, and a roughness of not more than 0.5 nm.
5. The hamburger type ceramic-crystal composite substrate of claim 1, wherein the low temperature sintered ceramic sheet (1) is one of an oxide ceramic, a fluoride ceramic, and a metal oxide ceramic.
6. The hamburger type ceramic-crystal composite substrate of claim 1 wherein the nanocrystalline chip (2) is one of sapphire, monocrystalline silicon, gallium arsenide, gallium nitride, silicon carbide.
7. A method of preparing a "hamburger" ceramic-crystal composite substrate of any of claims 1-6, comprising the steps of:
step S 1 : preparing a ceramic sheet (1) and a nanocrystal sheet (2) sintered at low temperature, polishing the bonding surface, and wiping the bonding surface by using a cleaning wiper to remove organic impurities;
step S 2 : ultrasonic cleaning is carried out on the ceramic sheet (1) and the nano crystal sheet (2) after the wiping treatment to remove the residual abrasive particles, dissolved residues and organic matters on the bonding surface; placing the ceramic sheet (1) and the nano crystal sheet (2) in a baking oven, and baking under the conditions that the baking temperature is 45-190 ℃ and the baking time is 2.5-6 h;
step S 3 : immersing the dried ceramic sheet (1) and the dried nanocrystal sheet (2) in a mixed acid solution with the volume ratio of sulfuric acid to phosphoric acid=1:5.5 and the concentration of 12-21% for 15-45 min, and removing oxides on the surfaces of the ceramic sheet (1) and the nanocrystal sheet (2); then, the mixture is washed by deionized water and soaked in cyclohexane solution to isolate air;
step S 4 : placing the ceramic sheet (1) and the nanocrystal sheet (2) together with cyclohexane solution in a plasma cleaning machine, and adding a concentrateThe bonding surfaces of the ceramic sheet (1) and the nanocrystal sheet (2) are cleaned and activated by using an ethylenediamine tetraacetic acid activator with the density of 5 mmol/l;
step S 5 : the bonding interface material is diluted and then is uniformly coated or sprayed on the bonding surfaces of the ceramic sheet (1) and the nano crystal sheet (2) to form a bonding material layer (3), the bonding surfaces of the ceramic sheet (1) and the nano crystal sheet (2) are tightly adhered and are pressed and fixed by using a graphite clamp (4), and the clamping pressure is 12-32 Kg/cm 2 The dwell time is 1-4 h, and a composite substrate sample is prepared;
step S 6 : placing the composite substrate sample with pressure maintaining in a vacuum hot pressing furnace for heat treatment;
step S 7 : and taking out the composite substrate sample subjected to heat treatment from the vacuum hot pressing furnace, and opening the graphite clamp (4) to obtain the composite substrate (6) formed by bonding the ceramic sheet (1) and the nano crystal sheet (2).
8. The method for preparing a "hamburger" ceramic-crystal composite substrate of claim 7, wherein step S 6 The heat treatment specifically comprises the following steps:
step S 61 : heating the composite substrate sample to an annealing temperature of 70-600 ℃ at a heating rate of 5-7 ℃/min, and an annealing time of 20-70 h;
step S 62 : the material sample after the annealing treatment is cooled to room temperature at a cooling rate of 3-5 ℃/min.
9. The method for producing a ceramic-single crystal composite substrate according to claim 7, wherein step S 5 The medium bonding interface diluting material specifically comprises the following steps:
step S 51 : weighing and mixing the powder in a proportion uniformly, feeding the powder mixture into a crystal slurry thickener for thickening, and enabling the crystal slurry after thickening to flow into a centrifugal machine through a circular pipe in a gravity flow mode for solid-liquid separation to obtain a bonding interface material with high purity;
step S 52 : diluting the bonding interface material with any one of absolute ethyl alcohol, distilled water or deionized water, and diluting at stirring speed of 130-350 r/min for 15-25 min.
10. The method for preparing a "hamburger" ceramic-crystal composite substrate of claim 7, wherein step S 1 Or step S 2 The cleaning solution is a mixed solution composed of deionized water, absolute ethyl alcohol and acetone.
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