CN101462169A - Method for preparing aluminium nitride substrate - Google Patents
Method for preparing aluminium nitride substrate Download PDFInfo
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- CN101462169A CN101462169A CNA2007101611197A CN200710161119A CN101462169A CN 101462169 A CN101462169 A CN 101462169A CN A2007101611197 A CNA2007101611197 A CN A2007101611197A CN 200710161119 A CN200710161119 A CN 200710161119A CN 101462169 A CN101462169 A CN 101462169A
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Abstract
The invention relates to a method for preparing an aluminum nitride substrate. The method comprises the following steps: a) most aluminum nitride (AlN) particles are evenly covered on the surface of an aluminum substrate first; b) the aluminum substrate is sent to a vacuum furnace; ammonia gas (NH3) is conducted to the vacuum furnace; and c) the aluminum substrate in the vacuum furnace is heated; therefore, the aluminum nitride substrate is obtained in the vacuum furnace. The vacuum furnace has the following set condition: the temperature range of the furnace is between 400 and 580DEG C.
Description
Technical field
The present invention is relevant with the metal material surface treatment technology, particularly relevant for a kind of method for preparing aluminium nitride substrate.
Background technology
The known method for preparing aluminium nitride substrate mainly can be divided into following two kinds:
One, burning method (co-fire) altogether is that a metal paste that is mixed with refractory metal is coated an aluminium base surface, carry out sintering with the above high temperature of 1700 degree Celsius again, to form an aln layer that is positioned at this aluminium base surface, reach the purpose of preparation aluminium nitride substrate; The characteristic of burning method altogether is that aln layer can be coated on the aluminium base surface with higher bond strength.Yet because this kind mode is the long-time continuous high temperature sintering, the peripheral part of aluminium base is shunk crooked easily in the process of sintered aluminum nitride layer and is out of shape, and has the not good problem of yield.
Two, back burning method (post-fire) is carried out sintering with the above high temperature of 1700 degree Celsius equally; Its difference is: back burning method is divided into sintering process carries out for several times, and then overcomes aluminium base and produce the problem of distortion in the long-time continuous high temperature sintering.Yet this kind mode will be derived the aln layer bond strength compared to the low problem of the method for burning altogether, have the not good problem of yield equally.
For addressing the above problem, number No. 200618203 patent " manufacture method of metallization aluminium nitride substrate and the substrate of gained " thus as the TaiWan, China patent disclosure, it mixes a metal paste and a sintering aid that is mixed with refractory metal, coats an aluminium base surface again; At last, to the temperature of 1900 degree Celsius aluminium base was carried out sintering 30 minutes to 24 hours, make the aluminium base surface form an aln layer, can obtain an aluminium nitride substrate with 1700 degree Celsius.Wherein, above-mentioned refractory metal is selected from tungsten and molybdenum is wherein a kind of, and it is wherein a kind of that this sintering aid is selected from the compound of the compound of rare earth metal and alkaline-earth metal.
Yet said method all carries out high temperature sintering more than 1700 degree Celsius, and procedure of processing complicated outside, moreover the shortcoming of long processing time is arranged, therefore very expend the energy; High temperature sintering simultaneously like this also is easy to generate the problem of thermal deformation.
In sum, the known method for preparing aluminium nitride substrate has above-mentioned disappearance and haves much room for improvement.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing aluminium nitride substrate, it is for the low temperature method for making and can simplify procedure for processing, has the characteristic that shortens process time, and can save the energy.
Another purpose of the present invention is to provide a kind of method for preparing aluminium nitride substrate, its energy cryogenic forming, the problem of minimizing thermal deformation.
For achieving the above object, the method for preparing aluminium nitride substrate provided by the invention comprises following each step:
A) earlier with most aluminium nitride (AlN) uniform particles cover in an aluminium base surface;
B) this aluminium base is sent in the vacuum drying oven, again to feeding ammonia (NH in this vacuum drying oven
3); And
C) this aluminium base in this vacuum drying oven is heated, can in this vacuum drying oven, obtain an aluminium nitride substrate;
Imposing a condition of this vacuum drying oven is as follows: temperature range is 400 degree Celsius～580 degree Celsius in the stove.
The described method for preparing aluminium nitride substrate, wherein, described this aluminium base of step a) is handled through a previous operations before processing in advance, and this previous operations comprises following program:
A1) earlier this aluminium base is heat-treated and planarizing process;
A2) remove oxide, greasy dirt and the spot on this aluminium base surface with ultrasonic;
A3) clean this aluminium base surface with pure water, the resistance value of pure water is more than 10K Ω (Ao Mu); And
A4) remove the moisture on this aluminium base surface in the low temperature drying mode.
The described method for preparing aluminium nitride substrate, wherein, described those aluminum nitride particles of step a) are selected from direct placement, Hpdc and handle and liquid state is adhered to wherein a kind of mode of processing and covered in this aluminium base surface.
The described method for preparing aluminium nitride substrate, wherein, the described liquid state of step a) is adhered to processing and is comprised following program:
A1) earlier to this aluminium base surface coating one metal cream, this metal cream is selected from aluminium cream and indium cream is wherein a kind of; And
A2) make those aluminum nitride particles be attached to this metal cream again, those aluminum nitride particles are covered in the purpose on this aluminium base surface to reach indirectly.
The described method for preparing aluminium nitride substrate, wherein, described those aluminum nitride particles of step a) are with self propagation high-temperature synthesis (self-propagating high-temperature synthesis; SHS) made.
The described method for preparing aluminium nitride substrate, wherein, described respectively this aluminum nitride particle of step a) is a nano-scale particle.
The described method for preparing aluminium nitride substrate, wherein, described respectively this aluminum nitride particle of step a) is 10～40 nanometers.
The described method for preparing aluminium nitride substrate, wherein, the described ammonia purity of step b) is more than 99%.
The described method for preparing aluminium nitride substrate, wherein, in the step c), press in the chamber of this vacuum drying oven is the following vacuum pressures of 5 milli-torrs (milliTorr).
The described method for preparing aluminium nitride substrate, wherein, temperature range is preferably 550 degree Celsius in described this stove of step c).
The described method for preparing aluminium nitride substrate, wherein, step c) described should heat time heating time scope be preferably 1 hour～5 hours.
The described method for preparing aluminium nitride substrate wherein, also comprises a step d) and takes out this aluminium nitride substrate and move to outside the stove from this vacuum drying oven and cool off.
The described method for preparing aluminium nitride substrate, wherein prepared this aluminium nitride substrate includes:
One aluminium base; And
One is formed at the aln layer on this aluminium base surface.
Aluminium nitride substrate provided by the invention includes:
One aluminium base; And
One is formed at the aln layer on this aluminium base surface.
Described prepared this aln layer of method for preparing aluminium nitride substrate is formed with sintering processing by most aluminum nitride particles, and respectively this aluminum nitride particle is a nano-scale particle.
The described method for preparing aluminium nitride substrate, wherein, respectively this aluminum nitride particle is 10～40 nanometers.
The described method for preparing aluminium nitride substrate, wherein, those aluminum nitride particles are with self propagation high-temperature synthesis (self-propagating high-temperature synthesis; SHS) made.
Prepare the method for aluminium nitride substrate by the present invention, by above-mentioned steps, it utilizes ammonia that this aluminium base is carried out nitrogenize and replaces known sintering aid, and can process under the cryogenic conditions of 400 degree Celsius～580 degree Celsius with temperature in the stove; This kind mode can make relative this aluminium base of this aln layer have higher adhesive strength, overcomes this aluminium base simultaneously because of the problem of sintering temperature up to the above easy deformation of 1700 degree Celsius.Moreover the present invention can simplify the formality of this aluminium nitride substrate of preparation, has the characteristic that shortens process time.
Description of drawings
Fig. 1 is the action flow chart of the present invention's first preferred embodiment.
Fig. 2 is the structural representation of the present invention's first preferred embodiment, mainly discloses the preceding situation of aluminium base processing.
Fig. 3 mainly discloses aluminum nitride particle and covers in the state of aluminium base end face for the structural representation of the present invention's first preferred embodiment.
Fig. 4 mainly discloses the processing situation of aluminium base in vacuum drying oven for the processing schematic diagram of the present invention's first preferred embodiment.
Fig. 5 is the structural representation of the present invention's first preferred embodiment, mainly discloses the structure of aluminium nitride substrate, i.e. situation after the aluminium base processing.
Fig. 6 is the structural representation of the present invention's second preferred embodiment, mainly discloses aluminum nitride particle and covers enforcement aspect in the aluminium base surface in the Hpdc mode.
Fig. 7 is the structural representation of the present invention's second preferred embodiment, mainly discloses the structure of aluminium nitride substrate, i.e. situation after the aluminium base processing.
Fig. 8 is the structural representation of the present invention's the 3rd preferred embodiment, mainly discloses the preceding situation of aluminium base processing.
Fig. 9 is the structural representation of the present invention's the 3rd preferred embodiment, mainly discloses the situation behind the aluminium base coating metal cream.
Figure 10 mainly discloses the situation that aluminum nitride particle covers for the structural representation of the present invention's the 3rd preferred embodiment.
Figure 11 is the structural representation of the present invention's the 3rd preferred embodiment, mainly discloses the structure of aluminium nitride substrate, i.e. situation after the aluminium base processing.
Primary clustering symbol description in the accompanying drawing:
Aluminium base (10)
Aluminum nitride particle (20)
Vacuum drying oven (30)
Aluminium nitride substrate (40)
Aln layer (50)
Aluminium base (60)
Aluminum nitride particle (70)
Aluminium nitride substrate (80)
Aln layer (90)
Aluminium base (100)
Metal cream (102)
Aluminum nitride particle (1T0)
Aluminium nitride substrate (120)
Aln layer (130)
The specific embodiment
The present invention prepares the method for aluminium nitride substrate, comprises following each step: a) earlier with most aluminium nitride (AlN) uniform particles cover in an aluminium base surface; B) this aluminium base is sent in the vacuum drying oven, again to feeding ammonia (NH in this vacuum drying oven
3); C) this aluminium base in this vacuum drying oven is heated, can in this vacuum drying oven, obtain an aluminium nitride substrate; Imposing a condition of this vacuum drying oven is as follows: temperature range is 400 degree Celsius～580 degree Celsius in the stove.
In order to describe feature of the present invention and effect place in detail, lift following preferred embodiment and conjunction with figs. the explanation as after, wherein:
See also Fig. 1 to Fig. 5, be a kind of method for preparing aluminium nitride substrate that the present invention's first preferred embodiment is provided, it comprises following each step:
A) aluminium base (10) is handled through a previous operations before processing in advance, comprises following program:
A1) earlier this aluminium base (10) is heat-treated and planarizing process;
A2) remove this aluminium base (10) surperficial oxide, greasy dirt and spot with ultrasonic;
A3) clean this aluminium base (10) surface with pure water, the resistance value of pure water is more than 10K Ω (Ao Mu); And
A4) remove the surperficial moisture of this aluminium base (10) in the low temperature drying mode.
See also Fig. 2 to Fig. 3, earlier most aluminium nitride (AlN) particles (20) are covered equably in the end face of this aluminium base (10); Those aluminum nitride particles (20) are with self propagation high-temperature synthesis (self-propagating high-temperature synthesis; SHS) made nano-grade size particle, respectively the diameter of this aluminum nitride particle (20) is about 10 nanometers～40 nanometers; In other words, the specific area of nano-grade size particle (specific surface area) is big compared to the specific area of general particle; Therefore use the nano-grade size particle to carry out sintering, it helps aluminium nitride densified and reduce needed sintering temperature in the processing procedure when sintering, and then can show special characteristic and function aspect processing.
B) see also Fig. 4, this aluminium base (10) is sent in the vacuum drying oven (30), to feeding ammonia in this vacuum drying oven (30), its purity is at the ammonia (NH more than 99% again
3) be preferable; In the present embodiment, the concentration of ammonia is 99.9%.
C) this aluminium base (10) in this vacuum drying oven (30) is heated, ammonia can disengage this aluminium base (10) needed activated nitrogen atom when carrying out nitrogenize (nitriding) because of decomposes; Wherein, part activated nitrogen atom can infiltrate this aluminium base (10) top layer, another part activated nitrogen atom can be attached to this aluminium base (10) surface, those activated nitrogen atoms can produce bond with the aluminum nitride particle of nano-grade size on this aluminium base (10) and reach the purpose of nitrogenize, to improve the case hardness of this aluminium base of metal (10).Imposing a condition of this vacuum drying oven (30) is as follows: temperature range is 400 degree Celsius～580 degree Celsius in the stove, is preferably 550 degree Celsius; The scope of heat time heating time is 1 hour～5 hours or also can more for a long time, certainly should heat time heating time relevant with the aluminium nitride thickness of formed thereby, thicker person is longer process time for desired thickness, be to be example with 2 hours the heat time heating time of present embodiment, the thicker person of desired thickness can form the above aluminium nitride thickness of 50um, if then can prolong process time; Press in the chamber of this vacuum drying oven (30) is the following vacuum pressures of 5 milli-torrs (milli Torr).See also Fig. 5, last, can in this vacuum drying oven (not shown), obtain an aluminium nitride substrate (40); This aluminium nitride substrate (40) has the aln layer (50) that this aluminium base (10) and is formed at this aluminium base (10) end face.Wherein, this aln layer (50) is formed by those aluminum nitride particle (not shown) sintering.
D) this vacuum drying oven (30) takes out this aluminium nitride substrate (40) and moves to stove and cools off outward certainly.
Thus, the method that the present invention prepares aluminium nitride substrate sees through above-mentioned steps, it utilizes ammonia that this aluminium base (10) is carried out nitrogenize and replaces known sintering aid, utilize the aluminum nitride particle of nano-grade size simultaneously, because tool special construction nano material, can produce and comprise skin effect, special optical property, thermal property, magnetic property and mechanical property etc. and the different effect of material habitually in the past, make and in utilization of the present invention, more can strengthen its bond effect, and under the cryogenic conditions of 400 degree Celsius～580 degree Celsius, can process with temperature in the stove; This kind mode can make this aln layer (50) relatively this aluminium base (10) have higher adhesive strength, overcome this aluminium base (10) simultaneously because of the problem of sintering temperature up to the above easy deformation of 1700 degree Celsius.Moreover the present invention can simplify the formality of this aluminium nitride substrate of preparation (40), has the characteristic that shortens process time, reduces the cost of this aluminium nitride substrate of preparation (40) simultaneously.
See also Fig. 6 and Fig. 7, a kind of method for preparing aluminium nitride substrate that the present invention's second preferred embodiment is provided, its step and first preferred embodiment are roughly the same; Its difference is: first preferred embodiment is the end face formation aln layer in aluminium base, and second preferred embodiment is the multiaspect formation aln layer in aluminium base, so its difference is described below:
A) aluminium base (60) is handled through a previous operations before processing in advance, and its program is identical with first preferred embodiment, does not give unnecessary details in this appearance.Most aluminum nitride particles (70) are covered equably in all surface of this aluminium base (60); Wherein, because those aluminum nitride particles (70) can't be reached the purpose that covers in the mode of direct placement for the lateral margin or the lower edge part of aluminium base (60).At this moment, those aluminum nitride particles (70) are selected from Hpdc and handle and liquid state is adhered to wherein a kind of mode of processing and covered in this aluminium base (60) surface.Present embodiment choosing is an example with the Hpdc processor, and the Hpdc processor is meant with high-pressure and pushes those aluminum nitride particles (70), those aluminum nitride particles (70) are directly adhered to and covers fully in this aluminium base (60) all surface.
The step b) of present embodiment to the step d) and first preferred embodiment discloses identical, do not give unnecessary details in this appearance.See also Fig. 7, be the prepared aluminium nitride substrate of present embodiment (80), this aluminium nitride substrate (80) has the aln layer (90) that this aluminium base (60) and is formed at this aluminium base (60) all surface, and this aln layer (90) is to be formed by those aluminum nitride particle (not shown) sintering.Thus, present embodiment can reach the effect that first preferred embodiment can be reached equally, and further discloses the present invention and how to process and to provide another enforcement aspect to this aluminium base (80) all surface.
See also Fig. 8 to Figure 11, a kind of method for preparing aluminium nitride substrate that the present invention's the 3rd preferred embodiment is provided, its step and second preferred embodiment are roughly the same; Its difference is: present embodiment is that choosing is adhered to the multiaspect formation aln layer of processing mode in aluminium base with liquid state, and it comprises following program:
A5) earlier to an aluminium base (100) surface coating one metal cream (102), this metal cream (102) is selected from aluminium cream and indium cream is wherein a kind of; In the present embodiment, this metal cream (102) choosing is an example with aluminium cream; And
A6) most aluminum nitride particles (110) are attached to this metal cream (102), those aluminum nitride particles (110) are covered fully in the purpose of this aluminium base (100) all surface to reach indirectly.
The step b) of present embodiment is identical with the first preferred embodiment those disclosed herein to step d), does not give unnecessary details in this appearance.See also Figure 11, be the prepared ㄧ aluminium nitride substrate of present embodiment (120), this aluminium nitride substrate (120) has the aln layer (130) that this aluminium base (100) and is formed at this aluminium base (100) all surface, and this aln layer (130) is to be formed by those aluminum nitride particle (not shown) sintering.Thus, present embodiment can reach the effect that second preferred embodiment can be reached equally, and another enforcement aspect is provided.
The present invention is disclosed constituent components and method step in aforementioned all embodiment, only for illustrating, is not to be used for limiting the scope of the invention, the alternative or variation of other equivalent elements or step, and the claim scope that also should be the present patent application contains.
Claims (17)
1, a kind of method for preparing aluminium nitride substrate comprises following each step:
A) earlier with most aluminium nitride (AlN) uniform particles cover in an aluminium base surface;
B) this aluminium base is sent in the vacuum drying oven, again to feeding ammonia (NH in this vacuum drying oven
3); And
C) this aluminium base in this vacuum drying oven is heated, can in this vacuum drying oven, obtain an aluminium nitride substrate;
Imposing a condition of this vacuum drying oven is as follows: temperature range is 400 degree Celsius～580 degree Celsius in the stove.
2, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, described this aluminium base of step a) is handled through a previous operations before processing in advance, and this previous operations comprises following program:
A1) earlier this aluminium base is heat-treated and planarizing process;
A2) remove oxide, greasy dirt and the spot on this aluminium base surface with ultrasonic;
A3) clean this aluminium base surface with pure water, the resistance value of pure water is more than 10K Ω (Ao Mu); And
A4) remove the moisture on this aluminium base surface in the low temperature drying mode.
3, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, described those aluminum nitride particles of step a) are selected from direct placement, Hpdc and handle and liquid state is adhered to wherein a kind of mode of processing and covered in this aluminium base surface.
4, according to the described method for preparing aluminium nitride substrate of claim 3, wherein, the described liquid state of step a) is adhered to processing and is comprised following program:
A1) earlier to this aluminium base surface coating one metal cream, this metal cream is selected from aluminium cream and indium cream is wherein a kind of; And
A2) make those aluminum nitride particles be attached to this metal cream again, those aluminum nitride particles are covered in the purpose on this aluminium base surface to reach indirectly.
5, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, described those aluminum nitride particles of step a) are with self propagation high-temperature synthesis (self-propagating high-temperaturesynthesis; SHS) made.
6, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, described respectively this aluminum nitride particle of step a) is a nano-scale particle.
7, according to the described method for preparing aluminium nitride substrate of claim 6, wherein, described respectively this aluminum nitride particle of step a) is 10～40 nanometers.
8, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, the described ammonia purity of step b) is more than 99%.
9, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, in the step c), press in the chamber of this vacuum drying oven is the following vacuum pressures of 5 milli-torrs (milliTorr).
10, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, temperature range is preferably 550 degree Celsius in described this stove of step c).
11, according to the described method for preparing aluminium nitride substrate of claim 1, wherein, step c) described should heat time heating time scope be preferably 1 hour～5 hours.
12,, wherein, also comprise a step d) and take out this aluminium nitride substrate and move to outside the stove from this vacuum drying oven and cool off according to the described method for preparing aluminium nitride substrate of claim 1.
13, according to the described method for preparing aluminium nitride substrate of claim 1, wherein prepared this aluminium nitride substrate includes:
One aluminium base; And
One is formed at the aln layer on this aluminium base surface.
14, a kind of aluminium nitride substrate includes:
One aluminium base; And
One is formed at the aln layer on this aluminium base surface.
15, according to described prepared this aln layer of method for preparing aluminium nitride substrate of claim 14, formed with sintering processing by most aluminum nitride particles, respectively this aluminum nitride particle is a nano-scale particle.
16, according to the described method for preparing aluminium nitride substrate of claim 15, wherein, respectively this aluminum nitride particle is 10～40 nanometers.
17, according to the described method for preparing aluminium nitride substrate of claim 15, wherein, those aluminum nitride particles are with self propagation high-temperature synthesis (self-propagating high-temperature synthesis; SHS) made.
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| CNA2007101611197A CN101462169A (en) | 2007-12-18 | 2007-12-18 | Method for preparing aluminium nitride substrate |
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| CNA2007101611197A CN101462169A (en) | 2007-12-18 | 2007-12-18 | Method for preparing aluminium nitride substrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106270509A (en) * | 2016-08-08 | 2017-01-04 | 武汉大学 | A kind of preparation method of Zinc oxide particles reinforced aluminum matrix composites |
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2007
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106270509A (en) * | 2016-08-08 | 2017-01-04 | 武汉大学 | A kind of preparation method of Zinc oxide particles reinforced aluminum matrix composites |
| CN106270509B (en) * | 2016-08-08 | 2018-09-07 | 武汉大学 | A kind of preparation method of Zinc oxide particles reinforced aluminum matrix composites |
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