CN106145068B - A kind of preparation method and aluminium nitride powder of high reflectance aluminium nitride powder - Google Patents
A kind of preparation method and aluminium nitride powder of high reflectance aluminium nitride powder Download PDFInfo
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- CN106145068B CN106145068B CN201510162233.6A CN201510162233A CN106145068B CN 106145068 B CN106145068 B CN 106145068B CN 201510162233 A CN201510162233 A CN 201510162233A CN 106145068 B CN106145068 B CN 106145068B
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Abstract
This application discloses a kind of high reflectance aluminum nitride powder preparation and aluminium nitride.Preparation method includes, and (a) presses AlN：Si3N4：Sr3N2：Ca3N2：EuN=1：0.27‑0.4：0‑0.3：0.03‑0.33：0 0.1 mole ratio, weigh raw material, and mole ratio AlN：Si3N4：(Sr3N2+Ca3N2+ EuN)=1：0.27‑0.4：0.3‑0.37；(b) grinding raw material mixes, and is calcined under nitrogen, and calcined product surface forms white powder；(c) white powder is collected, with absolute ethyl alcohol ultrasonic disperse, filtering, dries, obtains aluminium nitride.The preparation method of the application, using the production waste material in aluminiferous nitride system fluorescent material high temperature solid state reaction, the aluminium nitride powder of high-purity and high reflectance is prepared, application is expanded for aluminium nitride and prepares high heat conduction diffuse-reflective material and lay a good foundation.
Description
Technical field
The application is related to field of photovoltaic materials, more particularly to a kind of preparation method of high diffusing reflection rate aluminium nitride powder,
And its aluminium nitride powder prepared.
Background technology
Because the thermal conductivity of aluminium nitride is higher, it is possible to as a kind of heat filling or the material of heat-radiating substrate.But by
It is relatively low in the reflectivity of the aluminium nitride powder prepared at present, so typically being used not as a kind of diffuse-reflective material, but if can
So that the reflectivity of aluminium nitride to be improved, then a kind of diffuse-reflective material of high heat conduction can be made into.
Research shows that purity, oxygen content, particle diameter of aluminium nitride etc. can all impact to the reflectivity of aluminium nitride, high-purity
Degree, low oxygen content, the aluminium nitride powder reflectivity of fine grain are higher.But due to the preparation method such as metal of current aluminium nitride powder
The methods of Direct-Nitridation, alumina carbon thermal reduction, chemical vapor deposition, sol-gal process, aluminum nitride powder can not be avoided completely
The generation of impurity and oxygen in end, so as to cause the reflectivity of current aluminium nitride and other high diffusing reflection rate material presence very big
Gap, the use demand of diffuse-reflective material is not reached.
The content of the invention
The purpose of the application is to provide a kind of preparation method of new aluminium nitride so that the aluminium nitride of preparation has higher
Diffusing reflection rate.
The application employs following technical scheme：
This application discloses a kind of preparation method of high reflectance aluminium nitride powder, comprise the following steps,
(a) AlN is pressed：Si3N4：Sr3N2：Ca3N2：EuN=1：0.27-0.4：0-0.3：0.03-0.33：0-0.1 mole
Amount ratio, weighs AlN, Si3N4、Sr3N2、Ca3N2With EuN as raw material, and mole ratio AlN：Si3N4：(Sr3N2+Ca3N2+
EuN)=1：0.27-0.4：0.3-0.37；
(b) raw material for weighing step (a) are fully ground mixing, and high-temperature calcination is carried out under nitrogen protection atmosphere,
Until form white powder samples on the surface of calcined product；
(c) white powder samples caused by collection step (b), the white powder samples described in absolute ethyl alcohol ultrasonic disperse,
Then scattered suspension is filtered, dried, obtain the white powder of pure phase, i.e., described high reflectance aluminium nitride powder.
It should be noted that the key of the application is existing commercially available aluminium nitride and Si3N4、Sr3N2、
Ca3N2High-temperature calcination is carried out together with EuN, and one layer of white powder samples can be formed on the surface of its calcined product；The application creates
Property find, this layer of white powder samples are actually the aluminium nitride powder of high-purity, and the inside is contaminated with micro impurity, and nitrogen
It is widely different to change the particle diameter of aluminium powder body and impurity, can be separated；So as to prepare the aluminium nitride of high-purity and high reflectance
Powder.In the step of the application (c), EtOH Sonicate is scattered, filters and dries also precisely in order to removing the nitrogen that the removal of impurity obtains pure phase
Change aluminium.Confirmed in a kind of implementation of the application, as the commercially available aluminium nitride of raw material, its emissivity is only
82.6%, and the aluminium nitride powder that the preparation method processing Jing Guo the application obtains, its emissivity can be up to 91.8%.
It should also be noted that, " mole ratio AlN in the application：Si3N4：(Sr3N2+Ca3N2+ EuN)=1：0.27-
0.4：0.3-0.37 " is meant that, Sr3N2、Ca3N2Dosage with EuN three can be zero, but must be fulfilled for certain bar
Part；Illustrated exemplified by 1 mole of AlN is used in raw material, corresponding Sr3N2、Ca3N2Distinguish with the mole of EuN three
For 0-0.3 moles, 0.03-0.33 moles, 0-0.1 moles, that is to say, that the dosage of three can be respectively zero, still, must
Sr must be met3N2、Ca3N2With mole sum 0.3≤(Sr of EuN three3N2+Ca3N2+ EuN)≤0.37, that is to say, that
Sr3N2、Ca3N2Dosage with EuN three can not be zero simultaneously.
It should also be noted that, " with absolute ethyl alcohol ultrasonic disperse " its main purpose is to avoid hydrolysis of aluminium nitride, Ke Yili
Solution, other solvents that can be avoided hydrolysis of aluminium nitride and be easily removed are equally applicable to the application；In addition, ultrasonic disperse is also
A kind of mode of fairly simple effective dispersion powder, however not excluded that other process for dispersing can be used for the application.
Preferably, the condition of high-temperature calcination is the temperature more than 1800 DEG C, is sintered more than 6 hours.
It is furthermore preferred that the condition of high-temperature calcination is, at 1800 DEG C -2000 DEG C, 6-10 hours are sintered.
It should be noted that the purpose of the application is to carry out high-temperature calcination to raw material, form the surface of calcined product
One layer of white powder samples, required for the white powder samples are the application；As long as it is, therefore, to be understood that high-temperature calcination energy
Enough produce the white powder samples required for the application；In the preferred scheme of the application, in order to obtain the white of larger quantities
Color powder sample, while time cost is considered, especially its calcining heat and time are defined.
Preferably, raw material are weighed in step (a), is carried out in glove box of the water oxygen content less than 0.1ppm.
It should be noted that the purpose of the application is the final aluminium nitride powder for obtaining high reflectance, and oxygen content can be straight
Connecing influences the reflectivity of aluminium nitride powder, therefore, in the preferred scheme of the application, is preferably less than 0.1ppm in water oxygen content
Glove box in weigh raw material, and preferably, the operation such as be ground in glove box of the water oxygen content less than 0.1ppm,
Then rapidly load crucible, be transferred in atmosphere furnace and carry out high-temperature calcination.
Preferably, also include high-temperature calcination equipment is evacuated into 10 in advance in step (b)-1Below Pa, then it is re-filled with
Nitrogen carries out high-temperature calcination as protective atmosphere.
It should be noted that high-temperature calcination equipment is evacuated to 10-1Below Pa, also it is to try to avoid air from producing calcining
Raw white powder samples, i.e. aluminium nitride powder impact.
Preferably, the purity of raw material is more than 99.5% used by the application.
Preferably, the oxygen content of raw material is less than 0.5% used by the application.
It should be noted that the restriction of the purity and oxygen content to raw material, is to reduce white powder samples as far as possible
In impurity and oxygen content, improve the purity of the aluminium nitride powder of preparation as far as possible；It is appreciated that needed in more secondary production or use
In asking, the raw material outside the application restriction can also be used.
The another side of the application discloses aluminium nitride powder prepared by a kind of preparation method using the application.
The reflectivity of the aluminium nitride powder of the application is more than 90%.
It should be noted that according to existing preparation method, generally all there is more impurity or oxygen in the aluminium nitride of preparation,
So as to leverage the reflectivity of aluminium nitride powder, its reflectivity is substantially all only 80% or so, such as embodiments herein
In, the aluminium nitride reflectivity of purchase is only 82.6%；And the preparation method of the application can prepare high-purity and hypoxic
Aluminium nitride powder so that the reflectivity of aluminium nitride powder is up to 90%, and the aluminium nitride powder as prepared in the embodiment of the present application is anti-
It is 91.8% to penetrate rate, disclosure satisfy that the use demand of existing reflecting material；In the high thermal conductivity plus aluminium nitride in itself, for system
The diffuse-reflective material of standby high heat conduction is laid a good foundation.
Application of the aluminium nitride powder for simultaneously also disclosing the application again of the application in high heat conduction diffuse-reflective material.Can
To understand, first, aluminium nitride possesses high-termal conductivity in itself, secondly, the aluminium nitride powder that the preparation method by the application obtains,
Reflectivity greatly improves；Therefore, the aluminium nitride powder of the application can be used for preparing high heat conduction diffuse-reflective material.
The beneficial effect of the application is：
The preparation method of the high reflectance aluminium nitride powder of the application, overcome existing technology prejudice, creative utilization
Production waste material in the high temperature solid state reaction of aluminiferous nitride system fluorescent material, the aluminium nitride powder of high-purity is prepared, so as to
The reflectivity of prepared aluminium nitride powder is improved, is expansion application and the diffuse-reflective material of preparation high heat conduction of aluminium nitride
Lay a good foundation.
Brief description of the drawings
Fig. 1 is the X-ray diffraction analysis figure of the aluminium nitride prepared in the embodiment of the present application using the preparation method of the application；
In figure, A is the collection of illustrative plates of aluminium nitride prepared by embodiment, and B is aluminium nitride standard PDF cards, PDF76-0702.
Embodiment
During high-temperature solid phase reaction method prepares aluminiferous nitride system fluorescent material, it will usually in fluorescent material block
Surface forms one layer of white powder samples, and in fluorescent material production process, this layer of white powder is as production waste material or by-product
Product recovery uses；The application has found that this layer of white powder samples are actually high-purity by substantial amounts of production practices and research
The aluminium nitride powder of degree, so as to propose the preparation method of the application.
But in the production of normal high temperature solid state reaction generation aluminiferous nitride system fluorescent material, in order to obtain more
Good yield, is generally all to try to avoid or reduce the generation of white powder；The application is then just the opposite；Overcome existing technology
Prejudice, in preferable implementation, reaction raw materials, response area, reaction time and temperature etc. are optimized the application,
To obtain more white powders as far as possible.Wherein, in terms of response area, it will be understood that white powder is generated from fluorescence powder agglomates
Body surface face, therefore, increase response area, that is, increase the surface area of fluorescent material block, more white powder can be obtained naturally
End, the design of its specific response area, it can not limited herein depending on specific working condition.White powder samples
Produce the contact portion being prone in raw material and crucible, show as generating one layer of white powder in contact surface, i.e., it is high-purity
The aln layer with very high reflectance of degree, low oxygen content.It is also micro in white powder samples in addition to aluminium nitride
There is very big difference in fluorescent material, still, aluminium nitride and fluorescent material, can be separated by gas phase or liquid phase process on particle diameter,
So as to obtain the nano-grade size aluminium nitride powder of the high-purity high reflectance of pure phase；In a kind of implementation of the application preferably
Ultrasonic disperse is carried out in absolute ethyl alcohol.
The application is described in further detail below by specific embodiment.Following examples only are entered to advance to the application
One step illustrates, should not be construed as the limitation to the application.
Embodiment
The specific method that this example prepares high reflectance aluminium nitride powder is as follows：
(1) 2.9917g Sr is weighed in glove box of the water oxygen content less than 0.1ppm3N2, 0.0844g Ca3N2、
1.5349g Si3N4, 1.3454g AlN and 0.0436g EuN raw material, load crucible after being fully ground in mortar.
Wherein, raw material use the raw material that purity is less than 0.5% for more than 99.5%, oxygen content.
(2) crucible is transferred quickly in atmosphere furnace, is evacuated to 10-1Below Pa, nitrogen protection under normal pressure atmosphere is filled with,
1800 DEG C of sintering 8h.
(3) the top layer white powder samples of the fluorescent material block after sintering, the i.e. white powder containing particle fluorescence powder are taken
Layer, ultrasonic disperse is carried out using alcohol, suspension is filtered after the completion of scattered, dried, that is, obtains the high-purity of this example
Aluminium nitride.
Using X-ray diffraction analysis this example prepare aluminium nitride, its diffracting spectrum as shown in figure 1, by with aluminium nitride mark
Quasi- PDF cards PDF76-0702 carries out contrast and shown, aluminium nitride prepared by this example is single aluminium nitride phase, as pure nitridation
Aluminium.
Aluminium nitride powder prepared by this example, and the initial aluminium nitride powder as raw material, and alumina powder,
Reflectance test contrast is carried out under 444nm indigo plant laser, comparing result is as shown in table 1.
Reflectivity contrast under the aluminium nitride of table 1 and aluminum oxide 444nm blue lights
| Initial aluminium nitride | Synthesize aluminium nitride | Aluminum oxide | |
| Reflectivity | 82.6% | 91.8% | 97.5% |
As a result show, its emissivity of aluminium nitride prepared by this example is 91.8%, the initial aluminium nitride powder as raw material
Reflectivity is 82.6%, and the more initial aluminium nitride of aluminium nitride reflectivity prepared by this example improves more than 9%.Nitridation prepared by this example
Aluminium reflectivity is compared with aluminum oxide, and reflectivity is all more than 90%, it is seen that aluminium nitride prepared by this example can be led as a kind of height
The diffuse-reflective material of heat uses.
On the basis of being tested more than, this example is further tried high temperature solid state reaction reaction temperature and reaction time
Test, as a result show, reaction temperature sinters 8h or more long at 1800 DEG C or more, being capable of the more aluminium nitride of the amount of acquisition.
Above content is to combine the further description that specific embodiment is made to the application, it is impossible to assert this Shen
Specific implementation please is confined to these explanations.For the application person of an ordinary skill in the technical field, do not taking off
On the premise of conceiving from the application, some simple deduction or replace can also be made, should all be considered as belonging to the protection of the application
Scope.
Claims (10)
- A kind of 1. preparation method of high reflectance aluminium nitride powder, it is characterised in that：Comprise the following steps,(a) AlN is pressed：Si3N4：Sr3N2：Ca3N2：EuN=1：0.27-0.4：0-0.3：0.03-0.33：0-0.1 mole ratio Example, weighs AlN, Si3N4、Sr3N2、Ca3N2With EuN as raw material, and mole ratio AlN：Si3N4：(Sr3N2+Ca3N2+EuN) =1：0.27-0.4：0.3-0.37；(b) raw material for weighing step (a) are fully ground mixing, and high-temperature calcination is carried out under nitrogen protection atmosphere, until White powder samples are formed on the surface of calcined product；(c) white powder samples caused by collection step (b), the white powder samples described in absolute ethyl alcohol ultrasonic disperse, then Scattered suspension is filtered, dried, obtains the white powder of pure phase, i.e., described high reflectance aluminium nitride powder.
- 2. preparation method according to claim 1, it is characterised in that：The condition of the high-temperature calcination is, 1800 DEG C with On temperature, sinter more than 6 hours.
- 3. preparation method according to claim 1, it is characterised in that：The condition of the high-temperature calcination is, 1800 DEG C- 2000 DEG C, sinter 6-10 hours.
- 4. preparation method according to claim 1, it is characterised in that：Raw material are weighed in the step (a), in water oxygen Content is carried out in the glove box less than 0.1ppm.
- 5. preparation method according to claim 1, it is characterised in that：Also include in advance forging high temperature in the step (b) Burn equipment and be evacuated to 10-1Below Pa, nitrogen is then re-filled with as protective atmosphere, carries out high-temperature calcination.
- 6. according to the preparation method described in claim any one of 1-5, it is characterised in that：The purity of each raw material be 99.5% with On.
- 7. according to the preparation method described in claim any one of 1-5, it is characterised in that：The oxygen content of each raw material is less than 0.5%.
- A kind of 8. aluminium nitride powder prepared by preparation method using described in claim any one of 1-7.
- 9. aluminium nitride powder according to claim 8, it is characterised in that：The reflectivity of the aluminium nitride powder be 90% with On.
- 10. application of the aluminium nitride powder according to claim 8 or claim 9 in high heat conduction diffuse-reflective material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0733412A (en) * | 1993-07-19 | 1995-02-03 | Mitsui Toatsu Chem Inc | Production of aluminum nitride powder |
| CN1972883A (en) * | 2004-06-21 | 2007-05-30 | 株式会社德山 | Nitride sintered compact and method for production thereof |
| CN102502534A (en) * | 2011-11-18 | 2012-06-20 | 西安理工大学 | Preparation method of mesoporous AlN or GaN microparticle |
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- 2015-04-08 CN CN201510162233.6A patent/CN106145068B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0733412A (en) * | 1993-07-19 | 1995-02-03 | Mitsui Toatsu Chem Inc | Production of aluminum nitride powder |
| CN1972883A (en) * | 2004-06-21 | 2007-05-30 | 株式会社德山 | Nitride sintered compact and method for production thereof |
| CN102502534A (en) * | 2011-11-18 | 2012-06-20 | 西安理工大学 | Preparation method of mesoporous AlN or GaN microparticle |
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