CN109920725A - A kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate - Google Patents
A kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate, c-axis deviation within 10-20 °, with a thickness of 100-1000 microns, structure cell diameter 1-3 microns of nearly single crystal AlN transparent ceramic base preparation: pure AlN ceramic powder is fitted into polybag and forms cylinder and is put into warm equal pressing equipment and carries out compacting crushing, secondary compacting is cut into substrate disk and is put into sintering furnace high temperature sintering twice；C-axis orientating deviation is prepared in transparent ceramic base within 5 °, 5-100 microns of thickness of AlN or GaN quasi- monocrystalline layer: being prepared using the methods of molecular beam epitaxy or metal organic chemical compound vapor deposition method, high temperature sintering.Compound substrate prepared by the present invention can be realized epitaxial growth GaN or AlN monocrystal material or device, and buckling deformation is small, and thermal conductivity is high, and manufacturing cost is low, make it possible the production of 6 inches and 8 inches LED components.
Description
Technical field
The invention belongs to semiconductor material preparation field, it is related to a kind of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate
Preparation method.
Background technique
With the development and application of GaN or AlN base device technology, general illumination in the world and illumination field at present, base
This is monopolized by GaN or AlN base device.However, due to lacking GaN single crystal substrate, GaN base LED component mainly uses at present
Substrate material remains as AL2O3(sapphire) substrate is as main substrate material.Sapphire Substrate takes by development in recent years
Very big progress was obtained, however it still has very crucial problem and can not overcome, first, Sapphire Substrate and its extension
GaN or AlN material remains as hetero-epitaxy substrate, and the lattice mismatch of sapphire and GaN reach 13.6%, and thermal mismatching is more than 50%,
And the result of this problem is exactly after looking unfamiliar long GaN on a sapphire substrate, the universal warpage of epitaxial wafer is serious, and 4 inches of indigo plant is precious
Stone/GaN epitaxy piece angularity has just reached 200 microns or more, meanwhile, in order to overcome warpage, 4 inches of Sapphire Substrate is than 2
The Sapphire Substrate of inch has thickeied 1 times or more, sticks up only for the lattice mismatch and thermal mismatch stress bring that can balance GaN
Song, on this basis, the GaN device of saphire substrate material growth can not develop to 6 inches and 8 inches, because
Its sapphire thickness will increase more, while the warpage issues faced are almost that can not overcome.Meanwhile such problems is in indigo plant
It is even more serious when growing AIN on jewel substrate.Second, the thermal conductivity of Sapphire Substrate is very poor, about 25W/mk, and GaN now
Development with AlN base device increasingly develops towards the direction of power and miniaturization, and device power is higher and higher, and calorific value is got over
Come bigger, and Sapphire Substrate increasingly becomes the heat dissipation bottleneck of device, radiates unsmooth, the junction temperature that will lead to device quickly rises
Height, thus the problems such as causing component failure and service life to decline to a great extent.
From material system, use GaN single crystal or AlN monocrystalline as substrate be best solution route, firstly,
Perhaps AlN monocrystalline can be epitaxially grown as real isoepitaxial growth GaN single crystal or AlN monocrystal material GaN single crystal
GaN or AlN with epitaxial growth are homogeneous material, not any lattice mismatch and thermal mismatch problem, this is solved perfectly
The problem of increasing due to Sapphire Substrate and GaN or AlN extension bring stress problem and warpage and substrate thickness；It uses
Perhaps AlN single crystalline substrate growth GaN or AlN will not generate any warpage to GaN single crystal, so no matter substrate material is 2
It is very little, 4 cun or 6 cun, 8 cun, all do not need the problem of substrate material is thickeied to resist warpage.Secondly, GaN single crystal or AlN are mono-
Brilliant thermal conductivity is very high, can achieve 200W/mk or more, this perfectly solves that current device power is increasing and face again
The heat dissipation problem faced, therefore, GaN single crystal substrate or AlN single crystalline substrate are theoretically substrate materials the most perfect, however,
In actual industrial, preparing for GaN single crystal or AlN monocrystalline is extremely complex, and with high costs enables industry that can not receive, because
This, can not use always as commercial substrate.
Outside single crystalline substrate more than removing, AlN ceramic material, due to its material similar with GaN single crystal and AlN monocrystalline
Attribute is expected, so that people are easier to remember whether AlN ceramic can be used as substrate material use.Firstly, AlN ceramic
It is homogeneous material with GaN and AlN material, the lattice mismatch of AlN ceramic and GaN single crystal is only 2.4%, and thermal mismatching is only
5.2%, and it is zero with the lattice mismatch and thermal mismatching of AlN monocrystalline.Therefore, it is used as growth substrate, is there is no concern that appointing
What warpage issues and stress problem, meanwhile, the theoretical thermal conductivity of AlN ceramic can achieve 320W/mk, can be abundant
Meet GaN base and heat dissipation problem that AlN base device is faced.Therefore, consider from the meaning of this respect, AlN ceramic conduct
The substrate material use of GaN base and AlN base device is very suitable, however, existing AlN ceramic is single layer structure,
Only one layer of ceramics, AlN ceramic are ceramic property, and polycrystalline material, for grain size about at 3-5 microns, crystal orientation is disorderly and unsystematic, c-axis
Crystal orientation is disorderly arranged；And existing preparation AlN ceramic mainly uses tape casting technology, needs using colloid, diffusion
Agent and sintering aid: such as yttrium oxide, amount of impurities and content are high, can not form AlN crystalline ceramics structure.In Material growth
Under theoretical direction, mono-crystalline structures can not be grown on polycrystalline structure, and the impurity such as sintering aid serve as a contrast AlN ceramic
Bottom growth AlN monocrystalline or GaN single crystal have very big inhibition, therefore are existed using existing AlN ceramic growth GaN single crystal
It is theoretically impossible.
Summary of the invention
The object of the invention is exactly to solve the above-mentioned problems in the prior art, provides a kind of nearly monocrystalline Double-layered transparent AlN
The preparation method of Ceramic Composite substrate, the compound substrate of this method preparation can be realized extension close to the performance of AlN monocrystal material
GaN single crystal material or device or AlN monocrystal material or device are grown, buckling deformation is small, and thermal conductivity is high；And prepare the composite lining
The equipment cost at bottom is low, so that manufacturing cost is low, makes it possible the production of 6 inches and 8 inches LED components.
To achieve the above object, the technical solution of the invention is as follows: a kind of nearly monocrystalline Double-layered transparent AlN ceramic composite lining
The preparation method at bottom comprising following steps, nearly monocrystalline Double-layered transparent AlN ceramic compound substrate include the nearly single crystal AlN of lower layer
AlN the or GaN quasi- monocrystalline layer of transparent ceramic base and upper layer；The nearly single crystal AlN transparent ceramic base is with a thickness of 100-1000
Micron, structure cell diameter is free of sintering aid at 1-3 microns, and c-axis orientating deviation is within 10-20 °；The AlN or GaN is quasi-
Single crystalline layer is with a thickness of 5-100 microns, and c-axis orientating deviation is within 5 °；
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following steps:
(1) prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder；
(2) powder is formed using warm equal pressing forming technology: pure AlN ceramic powder is weighed first, be packed into polybag
Middle formation is cylindrical, tamps and seals；Then cylindrical plastic bag is put into warm equal pressing equipment, is 500-in pressure
2000MPa, temperature are 0.5-12H of pressure maintaining under conditions of 50-95 DEG C, and AlN powder has been pressed into cylinder at this time；
(3) the cylindrical plastic bag that AlN is housed is taken out, polybag is removed, cylindrical AlN is ground into partial size with pulverizer and is not surpassed
Cross the particulate matter of 1mm；Then the particulate matter is continued to be fitted into and forms cylinder in polybag, tamped and seal；Then by the circle
Cylindrical plastic bag is put into warm equal pressing equipment, is 500-2000MPa in pressure, temperature is pressure maintaining under conditions of 50-95 DEG C
0.5-12H, AlN powder has been pressed into cylinder at this time；
(4) the cylindrical plastic bag that AlN is housed is taken out, polybag is removed, molding AlN cylindrical body is cut, is cut into
With a thickness of multiple substrate disks of the nearly single crystal AlN transparent ceramic base thickness；
(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering temperature is 1700-1900 DEG C, and soaking time is
0.5—5H；After cooling to room temperature later, heating carries out double sintering again, and sintering temperature is 1800-2100 DEG C, soaking time
For 0.5-5H；Nearly single crystal AlN transparent ceramic base of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later,
When guaranteeing that temperature drops to 1600 DEG C at 1800-2100 DEG C when cooling, rate of temperature fall is no more than 1 DEG C/min；
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm
Below；
(2) molecular beam epitaxy MBE, metal organic chemical compound vapor deposition method MOCVD, hydride vapour phase epitaxy method are utilized
On HVPE, the nearly single crystal AlN transparent ceramic base substrate of pulse laser deposition PLD or physical vapor transport PVT after a polish
GaN the or AlN quasi- monocrystalline layer for growing the thickness forms the double-deck AlN crystalline ceramics substrate blank；
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, temperature rises to 1700-2000 DEG C
Afterwards, 0.5-2H is kept the temperature, then cools to room temperature, takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention.
It is further preferred that the AlN transparent ceramic base is with a thickness of 200-500 microns.
It is further preferred that AlN the or GaN quasi- monocrystalline layer is with a thickness of 10-50 microns.
It is further preferred that the step A(2) in, the dwell time in warm equal pressing equipment is 2-6H.
It is further preferred that the step B(2) in, it is saturating using the nearly single crystal AlN of molecular beam epitaxy MBE after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer is grown on bright ceramic substrate substrate, comprising the following steps: be put into sample
In MBE equipment, growth temperature is 1100-1400 DEG C, wherein preferably 1250 DEG C, growth time 20-300 minutes, and preferably 20-60
Minute.
It is further preferred that the step B(2) in, after a polish using metal organic chemical compound vapor deposition method MOCVD
Nearly single crystal AlN transparent ceramic base substrate on 5-100 microns of growth GaN or AlN single crystalline layer method, including following step
It is rapid: sample to be put into MOCVD device, growth temperature is 1100-1300 DEG C, wherein preferably 1250 DEG C, growth time 20-100
Minute, preferably 20-40 minutes.
It is further preferred that the step B(2) in, utilize the nearly monocrystalline of hydride vapour phase epitaxy method HVPE after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer is grown on AlN transparent ceramic base substrate, comprising the following steps: by sample
It is put into HVPE equipment, growth temperature is 900-1200 DEG C, wherein preferably 1150 DEG C, growth time 3-20 minutes, preferably 5-10
Minute.
It is further preferred that using on the nearly single crystal AlN transparent ceramic base substrate of pulse laser deposition PLD after a polish
The method of the GaN or AlN single crystalline layer of 5-100 microns of growth, comprising the following steps: sample is put into PLD equipment, growth temperature
Degree is 800-1200 DEG C, wherein preferably 1050 DEG C, growth time 5-100 minutes, and preferably 10-30 minutes, pulse laser wavelength
355nm, single pulse energy 200mj.
It is further preferred that the step B(2) in, utilize the nearly single crystal AlN of physical vapor transport PVT after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer is grown on transparent ceramic base substrate, comprising the following steps: put sample
Enter in PVT equipment, growth temperature is 800-1200 DEG C, wherein preferably 1050 DEG C, growth time 5-100 minutes, preferably 10-30
Minute.
The above method used twice warm equal pressing forming technology pure AlN ceramic powder is formed, do not add any
Powder body material will crush molding AlN by pulverizer, then carry out the static pressure such as secondary temperature for the first time after warm isostatic pressing
Molding, although particles of AlN powder itself can achieve within 1 micron, however, its cluster easy to form, when one-pass molding,
The porosity that centre is formed can be very high, and under such circumstances, the crystal grain for being unfavorable for sintering formation is close to each other, therefore, it is necessary to
The post forming after crushing, can be with effective solution stomata and fine and close problem, so that being conducive to sintering forms nearly mono-crystalline structures.On
The method of stating also uses the method for two-step sintering, does not use any sintering aid, at porcelain and reduces c-axis orientating deviation step by step；The
For once sintered temperature at 1700-1900 DEG C, sintering purpose is to make AlN substrate disk after molding into porcelain, reaches certain strong
Degree；After first sintering the grain size of AlN substrate disk will between 3-5 microns, meanwhile, c-axis orientation it is basic or miscellaneous
Disorderly without chapter, without the use of being once warming up to 2100 DEG C of sintering the reason of is that the temperature-fall period after first sintering is AlN
Ceramic crystalline grain merges into each other, and adjusts the critical process of phase transformation and curve.Second is sintered, sintering temperature at 1800-2100 DEG C,
So that AlN ceramic crystal grain merges into each other, to form unit cell dimension in 3 microns of c-axis orientating deviations below between 10-20 °
Nearly single crystal AlN transparent ceramic base.The present invention utilizes molecular beam epitaxy (MBE), metal organic chemical compound vapor deposition method
(MOCVD), the growths side such as hydride vapour phase epitaxy method (HVPE), pulse laser deposition (PLD), physical vapor transport (PVT)
After method growing AIN or GaN quasi- monocrystalline layer, crystal c axis orientation can achieve 10 ° or so, and high-temperature sintering process again, will
Realize that this layer of GaN's or AlN crystallizes self assembling process certainly again, c-axis orientation can achieve 5 degree or less.It is produced by the invention
Without impurity such as sintering aids in compound substrate, there is no growing AIN monocrystalline or GaN single crystal over the substrate are hindered because of impurity
The problem of；Compound substrate double-layer structure reduces c-axis deviation, the nearly single crystal AlN transparent ceramic base c-axis orientating deviation of lower layer step by step
Within 10-20 °, AlN the or GaN quasi- monocrystalline layer c-axis orientating deviation on upper layer is corrected to 5 degree ° hereinafter, mono- substantially close to AlN
The performance of brilliant material has reached the necessary condition of extension AlN monocrystalline or GaN single crystal material on upper layer, and buckling deformation is small, heat
Conductance is high；There are also the equipment cost for preparing the compound substrate is low, so that manufacturing cost is low, make 6 inches and 8 inches LED components
Production is possibly realized.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of compound substrate produced by the invention.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1, a kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate comprising following steps, closely
Monocrystalline Double-layered transparent AlN ceramic compound substrate includes the nearly single crystal AlN transparent ceramic base of lower layer and AlN or the GaN standard on upper layer
Single crystalline layer；For the nearly single crystal AlN transparent ceramic base with a thickness of 100 microns, structure cell diameter is free of sintering aid at 1 micron, and
C-axis orientating deviation is within 10-20 °；AlN the or GaN quasi- monocrystalline layer is with a thickness of 5 microns, and c-axis orientating deviation is within 5 °.
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following step
It is rapid: (1) to prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder.(2) it utilizes
Warm equal pressing forming technology forms powder: pure AlN ceramic powder being weighed first, is fitted into polybag and forms cylinder
Shape is tamped and is sealed；Then cylindrical plastic bag is put into warm equal pressing equipment, is 500MPa in pressure, temperature is 95 DEG C
Under conditions of pressure maintaining 0.5H, AlN powder has been pressed into cylinder at this time.(3) the cylindrical plastic bag that AlN is housed is taken out,
Polybag is removed, cylindrical AlN is ground into the particulate matter that partial size is no more than 1mm with pulverizer；Then the particulate matter is continued
It is fitted into polybag and forms cylinder, tamp and seal；Then the cylindrical plastic bag is put into warm equal pressing equipment, is being pressed
Power is 500MPa, and temperature is pressure maintaining 0.5H under conditions of 95 DEG C, and AlN powder has been pressed into cylinder at this time.(4) dress is taken out
There is the cylindrical plastic bag of AlN, removes polybag, molding AlN cylindrical body is cut, is cut into a thickness of the nearly list
Multiple substrate disks of brilliant AlN transparent ceramic base thickness.(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering
Temperature is 1800 DEG C, soaking time 5H；After cooling to room temperature later, heating carries out double sintering again, and sintering temperature is
1800 DEG C, soaking time 1H；It is transparent that nearly single crystal AlN of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later
Ceramic substrate guarantees temperature when cooling when dropping to 1600 DEG C for 1800 DEG C, and rate of temperature fall is no more than 1 DEG C/min.
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm or less；
(2) it utilizes on the nearly single crystal AlN transparent ceramic base substrate of molecular beam epitaxy MBE after a polish and grows the thickness
GaN or AlN quasi- monocrystalline layer forms the double-deck AlN crystalline ceramics substrate blank, comprising the following steps: sample is put into MBE equipment,
Growth temperature is 1100-1400 DEG C, wherein preferably 1250 DEG C, growth time 20-300 minutes, preferably 20-60 minutes；
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, after temperature rises to 1800 DEG C, protected
Warm 1H, then room temperature is cooled to, it takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention, as shown in Figure 1,1 is
The nearly single crystal AlN transparent ceramic base of lower layer, 2 be AlN the or GaN quasi- monocrystalline layer on upper layer.
Embodiment 2, a kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate comprising following steps, closely
Monocrystalline Double-layered transparent AlN ceramic compound substrate includes the nearly single crystal AlN transparent ceramic base of lower layer and AlN or the GaN standard on upper layer
Single crystalline layer；For the nearly single crystal AlN transparent ceramic base with a thickness of 500 microns, structure cell diameter is free of sintering aid at 3 microns, and
C-axis orientating deviation is within 10-20 °；AlN the or GaN quasi- monocrystalline layer with a thickness of 50 microns, c-axis orientating deviation 5 ° with
It is interior.
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following step
It is rapid: (1) to prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder.(2) it utilizes
Warm equal pressing forming technology forms powder: pure AlN ceramic powder being weighed first, is fitted into polybag and forms cylinder
Shape is tamped and is sealed；Then cylindrical plastic bag is put into warm equal pressing equipment, is 1500MPa in pressure, temperature is 60 DEG C
Under conditions of pressure maintaining 6H, AlN powder has been pressed into cylinder at this time.(3) the cylindrical plastic bag that AlN is housed is taken out, is gone
Except polybag, cylindrical AlN is ground into the particulate matter that partial size is no more than 1mm with pulverizer；Then the particulate matter is continued to fill
Enter and form cylinder in polybag, tamps and seal；Then the cylindrical plastic bag is put into warm equal pressing equipment, in pressure
For 1500MPa, temperature is pressure maintaining 6H under conditions of 60 DEG C, and AlN powder has been pressed into cylinder at this time.(4) it takes out and is equipped with
The cylindrical plastic bag of AlN removes polybag, molding AlN cylindrical body is cut, is cut into a thickness of the nearly monocrystalline
Multiple substrate disks of AlN transparent ceramic base thickness.(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering temperature
Degree is 1900 DEG C, soaking time 2H；After cooling to room temperature later, heating carries out double sintering, sintering temperature 2000 again
DEG C, soaking time 5H；Nearly single crystal AlN crystalline ceramics of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later
Substrate guarantees temperature when cooling when dropping to 1600 DEG C for 2000 DEG C, and rate of temperature fall is no more than 1 DEG C/min.
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm or less；
(2) using on the nearly single crystal AlN transparent ceramic base substrate of metal organic chemical compound vapor deposition method MOCVD after a polish
The method of the GaN or AlN single crystalline layer of 5-100 microns of growth, comprising the following steps: sample is put into MOCVD device, is grown
Temperature is 1100-1300 DEG C, wherein preferably 1250 DEG C, growth time 20-100 minutes, preferably 20-40 minutes；
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, after temperature rises to 1900 DEG C, protected
Warm 0.5H, then room temperature is cooled to, it takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention, as shown in Figure 1,1
It is AlN the or GaN quasi- monocrystalline layer on upper layer for the nearly single crystal AlN transparent ceramic base of lower layer, 2.
Embodiment 3, a kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate comprising following steps, closely
Monocrystalline Double-layered transparent AlN ceramic compound substrate includes the nearly single crystal AlN transparent ceramic base of lower layer and AlN or the GaN standard on upper layer
Single crystalline layer；With a thickness of 1000 microns, structure cell diameter is helped at 1.5 microns without sintering the nearly single crystal AlN transparent ceramic base
Agent, and c-axis orientating deviation is within 10-20 °；With a thickness of 10 microns, c-axis orientating deviation exists AlN the or GaN quasi- monocrystalline layer
Within 5 °.
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following step
It is rapid: (1) to prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder.(2) it utilizes
Warm equal pressing forming technology forms powder: pure AlN ceramic powder being weighed first, is fitted into polybag and forms cylinder
Shape is tamped and is sealed；Then cylindrical plastic bag is put into warm equal pressing equipment, is 1000MPa in pressure, temperature is 50 DEG C
Under conditions of pressure maintaining 2H, AlN powder has been pressed into cylinder at this time.(3) the cylindrical plastic bag that AlN is housed is taken out, is gone
Except polybag, cylindrical AlN is ground into the particulate matter that partial size is no more than 1mm with pulverizer；Then the particulate matter is continued to fill
Enter and form cylinder in polybag, tamps and seal；Then the cylindrical plastic bag is put into warm equal pressing equipment, in pressure
For 1000MPa, temperature is pressure maintaining 2H under conditions of 50 DEG C, and AlN powder has been pressed into cylinder at this time.(4) it takes out and is equipped with
The cylindrical plastic bag of AlN removes polybag, molding AlN cylindrical body is cut, is cut into a thickness of the nearly monocrystalline
Multiple substrate disks of AlN transparent ceramic base thickness.(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering temperature
Degree is 1700 DEG C, soaking time 0.5H；After cooling to room temperature later, heating carries out double sintering again, and sintering temperature is
1900 DEG C, soaking time 0.5H；It is saturating that nearly single crystal AlN of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later
Bright ceramic substrate guarantees temperature when cooling when dropping to 1600 DEG C for 1900 DEG C, and rate of temperature fall is no more than 1 DEG C/min.
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm or less；
(2) growth 5-on the nearly single crystal AlN transparent ceramic base substrate of hydride vapour phase epitaxy method HVPE after a polish is utilized
The method of 100 microns of GaN or AlN single crystalline layer, comprising the following steps: sample is put into HVPE equipment, growth temperature is
900-1200 DEG C, wherein preferably 1150 DEG C, growth time 3-20 minutes, preferably 5-10 minutes；
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, after temperature rises to 2000 DEG C, protected
Warm 2H, then room temperature is cooled to, it takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention, as shown in Figure 1,1 is
The nearly single crystal AlN transparent ceramic base of lower layer, 2 be AlN the or GaN quasi- monocrystalline layer on upper layer.
Embodiment 4, a kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate comprising following steps, closely
Monocrystalline Double-layered transparent AlN ceramic compound substrate includes the nearly single crystal AlN transparent ceramic base of lower layer and AlN or the GaN standard on upper layer
Single crystalline layer；For the nearly single crystal AlN transparent ceramic base with a thickness of 200 microns, structure cell diameter is free of sintering aid at 2 microns, and
C-axis orientating deviation is within 10-20 °；AlN the or GaN quasi- monocrystalline layer with a thickness of 100 microns, c-axis orientating deviation 5 ° with
It is interior.
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following step
It is rapid: (1) to prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder.(2) it utilizes
Warm equal pressing forming technology forms powder: pure AlN ceramic powder being weighed first, is fitted into polybag and forms cylinder
Shape is tamped and is sealed；Then cylindrical plastic bag is put into warm equal pressing equipment, is 2000MPa in pressure, temperature is 80 DEG C
Under conditions of pressure maintaining 12H, AlN powder has been pressed into cylinder at this time.(3) the cylindrical plastic bag that AlN is housed is taken out, is gone
Except polybag, cylindrical AlN is ground into the particulate matter that partial size is no more than 1mm with pulverizer；Then the particulate matter is continued to fill
Enter and form cylinder in polybag, tamps and seal；Then the cylindrical plastic bag is put into warm equal pressing equipment, in pressure
For 2000MPa, temperature is pressure maintaining 12H under conditions of 80 DEG C, and AlN powder has been pressed into cylinder at this time.(4) it takes out and is equipped with
The cylindrical plastic bag of AlN removes polybag, molding AlN cylindrical body is cut, is cut into a thickness of the nearly monocrystalline
Multiple substrate disks of AlN transparent ceramic base thickness.(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering temperature
Degree is 1750 DEG C, soaking time 3H；After cooling to room temperature later, heating carries out double sintering, sintering temperature 2100 again
DEG C, soaking time 3H；Nearly single crystal AlN crystalline ceramics of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later
Substrate guarantees temperature when cooling when dropping to 1600 DEG C for 2100 DEG C, and rate of temperature fall is no more than 1 DEG C/min.
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm or less；
(2) it is deposited using pulse laser and grows 5-100 microns on the nearly single crystal AlN transparent ceramic base substrate of PLD after a polish
GaN or AlN single crystalline layer method, comprising the following steps: sample is put into PLD equipment, growth temperature be 800-1200 DEG C,
Wherein, preferably 1050 DEG C, growth time 5-100 minutes, preferably 10-30 minutes, pulse laser wavelength 355nm, single pulse energy
200mj。
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, temperature rises to 1700 DEG C
Afterwards, 1.5H is kept the temperature, then cools to room temperature, takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention, such as Fig. 1
Shown, 1 is the nearly single crystal AlN transparent ceramic base of lower layer, and 2 be AlN the or GaN quasi- monocrystalline layer on upper layer.
Embodiment 5, a kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate comprising following steps, closely
Monocrystalline Double-layered transparent AlN ceramic compound substrate includes the nearly single crystal AlN transparent ceramic base of lower layer and AlN or the GaN standard on upper layer
Single crystalline layer；For the nearly single crystal AlN transparent ceramic base with a thickness of 350 microns, structure cell diameter is free of sintering aid at 2.5 microns,
And c-axis orientating deviation is within 10-20 °；AlN the or GaN quasi- monocrystalline layer with a thickness of 30 microns, c-axis orientating deviation 5 ° with
It is interior.
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following step
It is rapid: (1) to prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder.(2) it utilizes
Warm equal pressing forming technology forms powder: pure AlN ceramic powder being weighed first, is fitted into polybag and forms cylinder
Shape is tamped and is sealed；Then cylindrical plastic bag is put into warm equal pressing equipment, is 1300MPa in pressure, temperature is 70 DEG C
Under conditions of pressure maintaining 4H, AlN powder has been pressed into cylinder at this time.(3) the cylindrical plastic bag that AlN is housed is taken out, is gone
Except polybag, cylindrical AlN is ground into the particulate matter that partial size is no more than 1mm with pulverizer；Then the particulate matter is continued to fill
Enter and form cylinder in polybag, tamps and seal；Then the cylindrical plastic bag is put into warm equal pressing equipment, in pressure
For 1300MPa, temperature is pressure maintaining 4H under conditions of 70 DEG C, and AlN powder has been pressed into cylinder at this time.(4) it takes out and is equipped with
The cylindrical plastic bag of AlN removes polybag, molding AlN cylindrical body is cut, is cut into a thickness of the nearly monocrystalline
Multiple substrate disks of AlN transparent ceramic base thickness.(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering temperature
Degree is 1850 DEG C, soaking time 4H；After cooling to room temperature later, heating carries out double sintering, sintering temperature 1950 again
DEG C, soaking time 4H；Nearly single crystal AlN crystalline ceramics of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later
Substrate guarantees temperature when cooling when dropping to 1600 DEG C for 1950 DEG C, and rate of temperature fall is no more than 1 DEG C/min.
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm or less；
(2) micro- using growth 5-100 on the nearly single crystal AlN transparent ceramic base substrate of physical vapor transport PVT after a polish
The method of the GaN or AlN single crystalline layer of rice, comprising the following steps: sample is put into PVT equipment, growth temperature 800-1200
DEG C, wherein preferably 1050 DEG C, growth time 5-100 minutes, preferably 10-30 minutes；
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, after temperature rises to 1950 DEG C, protected
Warm 1.8H, then room temperature is cooled to, it takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention, as shown in Figure 1,1
It is AlN the or GaN quasi- monocrystalline layer on upper layer for the nearly single crystal AlN transparent ceramic base of lower layer, 2.
Above-described embodiment be only it is preferred and illustrative, those skilled in the art can do according to the description of this patent
Change with technology, is all covered by the protection scope of this patent.
Claims (10)
1. a kind of preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate, which is characterized in that it includes the following steps,
Nearly monocrystalline Double-layered transparent AlN ceramic compound substrate includes the nearly single crystal AlN transparent ceramic base of lower layer and the AlN or GaN on upper layer
Quasi- monocrystalline layer；With a thickness of 100-1000 microns, structure cell diameter is free of the nearly single crystal AlN transparent ceramic base at 1-3 microns
Sintering aid, and c-axis orientating deviation is within 10-20 °；AlN the or GaN quasi- monocrystalline layer is with a thickness of 5-100 microns, c-axis
Orientating deviation is within 5 °；
A, the preparation of nearly single crystal AlN transparent ceramic base of the c-axis deviation within 10-20 ° comprising following steps:
(1) prepare powder granule partial size within 1 micron, impurity content is lower than 0.1% pure AlN ceramic powder；
(2) powder is formed using warm equal pressing forming technology: pure AlN ceramic powder is weighed first, be packed into polybag
Middle formation is cylindrical, tamps and seals；Then cylindrical plastic bag is put into warm equal pressing equipment, is 500-in pressure
2000MPa, temperature are 0.5-12H of pressure maintaining under conditions of 50-95 DEG C, and AlN powder has been pressed into cylinder at this time；
(3) the cylindrical plastic bag that AlN is housed is taken out, polybag is removed, cylindrical AlN is ground into partial size with pulverizer and is not surpassed
Cross the particulate matter of 1mm；Then the particulate matter is continued to be fitted into and forms cylinder in polybag, tamped and seal；Then by the circle
Cylindrical plastic bag is put into warm equal pressing equipment, is 500-2000MPa in pressure, temperature is pressure maintaining under conditions of 50-95 DEG C
0.5-12H, AlN powder has been pressed into cylinder at this time；
(4) the cylindrical plastic bag that AlN is housed is taken out, polybag is removed, molding AlN cylindrical body is cut, is cut into
With a thickness of multiple substrate disks of the nearly single crystal AlN transparent ceramic base thickness；
(5) substrate disk is put into sintering furnace and carries out high temperature sintering, sintering temperature is 1700-1900 DEG C, and soaking time is
0.5—5H；After cooling to room temperature later, heating carries out double sintering again, and sintering temperature is 1800-2100 DEG C, soaking time
For 0.5-5H；Nearly single crystal AlN transparent ceramic base of the c-axis deviation obtained within the scope of 10-20 ° is taken out in cooling later,
When guaranteeing that temperature drops to 1600 DEG C at 1800-2100 DEG C when cooling, rate of temperature fall is no more than 1 DEG C/min；
B, AlN the or GaN quasi- monocrystalline layer is prepared in nearly single crystal AlN transparent ceramic base comprising following steps:
(1) the nearly single crystal AlN transparent ceramic base made is subjected to surface polishing treatment, surface polishing roughness reaches 1nm
Below；
(2) molecular beam epitaxy MBE, metal organic chemical compound vapor deposition method MOCVD, hydride vapour phase epitaxy method are utilized
On HVPE, the nearly single crystal AlN transparent ceramic base substrate of pulse laser deposition PLD or physical vapor transport PVT after a polish
GaN the or AlN quasi- monocrystalline layer for growing the thickness forms the double-deck AlN crystalline ceramics substrate blank；
(3) the double-deck AlN crystalline ceramics substrate blank is put into sintering furnace and carries out high temperature sintering, temperature rises to 1700-2000 DEG C
Afterwards, 0.5-2H is kept the temperature, then cools to room temperature, takes out and obtains nearly monocrystalline Double-layered transparent AlN ceramic compound substrate of the invention.
2. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 1, which is characterized in that
The step B(2) in, using being grown on the nearly single crystal AlN transparent ceramic base substrate of molecular beam epitaxy MBE after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer, comprising the following steps: sample is put into MBE equipment, growth temperature is
1100-1400 DEG C, growth time 20-300 minutes.
3. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 1, which is characterized in that
The step B(2) in, utilize the nearly single crystal AlN crystalline ceramics base of metal organic chemical compound vapor deposition method MOCVD after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer is grown on plate substrate, comprising the following steps: sample is put into MOCVD device
In, growth temperature is 1100-1300 DEG C, growth time 20-100 minutes.
4. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 3, which is characterized in that
The step B(2) in, utilize the nearly single crystal AlN crystalline ceramics base of metal organic chemical compound vapor deposition method MOCVD after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer is grown on plate substrate, comprising the following steps: sample is put into MOCVD device
In, growth temperature is 1250 DEG C, growth time 20-40 minutes.
5. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 1, which is characterized in that
The step B(2) in, using on the nearly single crystal AlN transparent ceramic base substrate of hydride vapour phase epitaxy method HVPE after a polish
The method of the GaN or AlN single crystalline layer of 5-100 microns of growth, comprising the following steps: sample is put into HVPE equipment, growth temperature
Degree is 900-1200 DEG C, growth time 3-20 minutes.
6. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 1, which is characterized in that
Using 5-100 microns of growth on pulse laser deposition PLD nearly single crystal AlN transparent ceramic base substrate after a polish GaN or
The method of AlN single crystalline layer, comprising the following steps: sample is put into PLD equipment, growth temperature is 800-1200 DEG C, when growth
Between 5-100 minutes, pulse laser wavelength 355nm, single pulse energy 200mj.
7. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 1, which is characterized in that
The step B(2) in, using being grown on the nearly single crystal AlN transparent ceramic base substrate of physical vapor transport PVT after a polish
The method of 5-100 microns of GaN or AlN single crystalline layer, comprising the following steps: sample is put into PVT equipment, growth temperature is
800-1200 DEG C, growth time 5-100 minutes.
8. the system of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate described according to claim 1 or 2 or 3 or 4 or 5 or 6 or 7
Preparation Method, which is characterized in that the A lN transparent ceramic base is with a thickness of 200-500 microns.
9. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 8, which is characterized in that
AlN the or GaN quasi- monocrystalline layer is with a thickness of 10-50 microns.
10. the preparation method of nearly monocrystalline Double-layered transparent AlN ceramic compound substrate according to claim 9, which is characterized in that
The step A(2) in, the dwell time in warm equal pressing equipment is 2H -6H.
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