CN101528638A - Process for producing aluminum nitride joint product - Google Patents
Process for producing aluminum nitride joint product Download PDFInfo
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- CN101528638A CN101528638A CNA2007800397781A CN200780039778A CN101528638A CN 101528638 A CN101528638 A CN 101528638A CN A2007800397781 A CNA2007800397781 A CN A2007800397781A CN 200780039778 A CN200780039778 A CN 200780039778A CN 101528638 A CN101528638 A CN 101528638A
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- aluminum nitride
- sintered product
- nitride sintered
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
- C04B37/005—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of glass or ceramic material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/04—Ceramic interlayers
- C04B2237/06—Oxidic interlayers
- C04B2237/064—Oxidic interlayers based on alumina or aluminates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/36—Non-oxidic
- C04B2237/366—Aluminium nitride
Abstract
This invention provides a process for producing an aluminum nitride joint product comprising aluminum nitride sinters joined to each other. The production process is characterized by comprising the step of disposing two aluminum nitride sinters having an alumina layer on their joining faces so that the joining faces face each other, interposing an alkaline earth metal compound-containing paste layer between the joining faces, and heating the assembly in this state at a temperature of 1300 to 1700 DEG C to join the aluminum nitride sinters to each other.
Description
Technical field
The present invention relates to the manufacture method of aluminum nitride bonded body.More particularly, the present invention relates to the be engaged with each other manufacture method of the aluminum nitride bonded body that forms of aluminum nitride sintered product.
Background technology
In recent years, in semiconductor-fabricating device, as the plate heater (plate heater) and the electrostatic chuck parts such as (electrostaticchuck) that are used to place with process semiconductor wafers, the parts that use the aluminium nitride by thermotolerance, excellent corrosion resistance to constitute.In the manufacturing of this parts that are made of aluminium nitride, a lot of situations are little aluminum nitride sintered product to be bonded with each other make big parts.Thus, can obtain to have the parts of different shape by the aluminum nitride sintered product of simple shape.
As the method for joining of aluminum nitride sintered product, known have a following method.For example, in patent documentation 1, as shown in Figure 5, coating comprises the paste 502 of the powder of aluminium nitride powder and rare earth oxide and/or lime carbonate on aluminum nitride sintered product 501, and paste aluminum nitride sintered product 503 thereon, on the A direction, apply 1～250kgf/cm then
2Pressure, and be heated to 1700～2000 ℃, make aluminum nitride bonded body 500.In addition, in patent documentation 2, use the joint compound of the powder of the oxide powder comprise aluminium nitride powder, basic metal or alkaline-earth metal and rare earth oxide, at 5～500kgf/cm
2Pressure under, in first operation, be heated to 1400～1650 ℃, in second operation, be heated to 1650～1800 ℃, aluminum nitride sintered product is engaged with each other.
Patent documentation 1: Japanese kokai publication hei 11-157951 communique
Patent documentation 2: Japanese kokai publication hei 10-273370 communique
Summary of the invention
The problem that invention will solve
Yet in order to obtain the conjugant of firm engagement, the firing temperature when any of these method of joining all needs to make with aluminum nitride sintered product is with the Heating temperature of degree.Because the heating under this high temperature, aluminum nitride sintered product might go bad, distortion etc.In addition, these method of joining any, all need to apply heating and pressure, this is a trouble.
Therefore, the purpose of this invention is to provide a kind of can lesser temps under atmospheric pressure under with firm engagement, aluminum nitride bonded body the each other manufacture method of aluminum nitride sintered product.
The method that is used to deal with problems
The inventor etc. further investigate in order to address the above problem, and found that, by using specific aluminum nitride sintered product, aluminum nitride sintered product can be engaged each other securely, thereby finish the present invention.
That is to say, the manufacture method of aluminum nitride bonded body of the present invention is with the be engaged with each other manufacture method of the aluminum nitride bonded body that forms of aluminum nitride sintered product, it is characterized in that, comprise following joint operation: be in above-mentioned junction surface relatively and exist between the above-mentioned junction surface under the state of the paste layer that comprises alkaline earth metal compound at two above-mentioned aluminum nitride sintered products that are formed with alumina layer on the junction surface, under 1300～1700 ℃ temperature, heat, above-mentioned aluminum nitride sintered product is engaged with each other.
Above-mentioned joint operation is preferably following joint operation: form the paste layer that comprises alkaline earth metal compound on the junction surface that is formed with alumina layer of an aforementioned aluminum nitride sintered product, and with the junction surface that is formed with alumina layer of another aforementioned aluminum nitride sintered product attached on this paste layer, under 1300～1700 ℃ temperature, heat then, above-mentioned aluminum nitride sintered product is engaged with each other.
The thickness of formed alumina layer is preferably 0.1～10 μ m on the junction surface of above-mentioned aluminum nitride sintered product.
The invention effect
According to the manufacture method of aluminum nitride bonded body of the present invention, can under the lesser temps under atmospheric pressure aluminum nitride sintered product be engaged each other securely.
Description of drawings
Fig. 1 is the figure that is used to illustrate the manufacture method of aluminum nitride bonded body of the present invention.
Fig. 2 is the figure that is used to illustrate the manufacture method of aluminum nitride bonded body of the present invention.
Fig. 3 is the figure that is used to illustrate the manufacture method of aluminum nitride bonded body of the present invention.
Fig. 4 is the figure that is used to illustrate the manufacture method of aluminum nitride bonded body of the present invention.
Fig. 5 is the figure that is used to illustrate the manufacture method of aluminum nitride sintered product in the past.
Fig. 6 is the photo of joint interface of an example of aluminum nitride bonded body of the present invention.
Fig. 7 is the figure that is used to illustrate the measuring method of bond strength.
Fig. 8 is the figure of manufacture method that is used for illustrating the conjugant of embodiment.
Fig. 9 is the figure of manufacture method that is used for illustrating the conjugant of embodiment.
Figure 10 is the figure of manufacture method that is used for illustrating the conjugant of embodiment.
Figure 11 is the figure of manufacture method that is used for illustrating the conjugant of embodiment.
Description of reference numerals
101: aluminum nitride sintered product
102: the junction surface
103: alumina layer
201: the paste layer
301: aluminum nitride sintered product
302: the junction surface
303: alumina layer
400: aluminum nitride bonded body
401: the junction surface
500: aluminum nitride bonded body
501: aluminum nitride sintered product
502: paste
503: aluminum nitride sintered product
A: the direction that pressure applies
Embodiment
Below describe the present invention in detail.
The manufacture method of aluminum nitride bonded body of the present invention is with the be engaged with each other manufacture method of the aluminum nitride bonded body that forms of aluminum nitride sintered product, comprise joint operation as described below: be in above-mentioned junction surface at two above-mentioned aluminum nitride sintered products that are formed with alumina layer on the junction surface and heat relatively and under the state that has the paste layer that comprises alkaline earth metal compound between the above-mentioned junction surface, thereby above-mentioned aluminum nitride sintered product is engaged with each other.It is desirable to, in above-mentioned joint operation, on the junction surface that is formed with alumina layer of an above-mentioned aluminum nitride sintered product, form the paste layer that comprises alkaline earth metal compound, and with the junction surface that is formed with alumina layer of another above-mentioned aluminum nitride sintered product attached on this paste layer, heating is engaged with each other above-mentioned aluminum nitride sintered product then.
Like this, in manufacture method of the present invention, on the junction surface of aluminum nitride sintered product, be formed with alumina layer, therefore under lower temperature and normal atmosphere, this sintered compact can be engaged each other securely.In addition, the gained conjugant has high resistance to air loss.
Be described more specifically manufacture method of the present invention with bottom with reference to the accompanying drawing limit.
At first, in above-mentioned joint operation, as shown in Figure 1, prepare on junction surface 102, to be formed with the aluminum nitride sintered product 101 of alumina layer 103.
Being shaped as of aluminum nitride sintered product 101 is tabular, but the invention is not restricted to this, for example, can be cylindric, polygonal column etc.In addition, aluminum nitride sintered product can be that hollow structure also can be a solid construction.Can suitably select the shape of aluminum nitride sintered product, so that obtain the structure of required conjugant.
The relative density of aluminum nitride sintered product 101 is preferably more than 97%.
In addition, the thickness of alumina layer 103 is preferably 0.1～10 μ m, and more preferably 1～5 μ m is an ideal.The thickness of alumina layer is crossed when approaching, and can not obtain the effect of manufacture method of the present invention sometimes.When the thickness of alumina layer was blocked up, the bond strength between alumina layer and the aluminum nitride sintered product sometimes can reduce.
The manufacture method that is formed with the aluminum nitride sintered product 101 of alumina layer 103 on junction surface 102 does not have specific limited, for example, can be listed below describedly after making aluminum nitride sintered product, is becoming the method that forms alumina layer on the surface on junction surface.
In the manufacturing of aluminum nitride sintered product, at first, in aluminium nitride powder, add organic binder bond, as required, further add sintering aid, dispersion agent, dispersion medium etc., mix preparation slurry or paste.
As organic binder bond, can enumerate acrylic resins such as butyral resin, poly-n-butyl methacrylate such as polyvinyl butyral acetal etc.The aluminium nitride powder of per 100 weight parts, this organic binder bond are usually with 0.1～30 weight part, preferably use with the amount of 1～15 weight part.
As sintering aid, can enumerate alkaline earth series oxide compound, Y such as CaO, SrO
2O
3, CeO
2, Ho
2O
3, Yb
2O
3, Gd
2O
3, Nd
2O
3, Sm
2O
3, Dy
2O
3Deng rare earth is oxide compound.In the middle of these, the suitable Y that uses
2O
3In addition, sintering aid may not be an oxide compound, for example can be carbonate, nitrate, phosphoric acid salt etc.The aluminium nitride powder of per 100 weight parts, this sintering aid are usually with 0.1～30 weight part, preferably use with the amount of 1～15 weight part.
As dispersion agent, can enumerate glycerol compounds class etc.The aluminium nitride powder of per 100 weight parts, this dispersion agent are usually with 0.1～10 weight part, preferably use with the amount of 0.5～5 weight part.
As dispersion medium, can enumerate ethanol.The aluminium nitride powder of per 100 weight parts, this dispersion medium are usually with 10～50 weight parts, preferably use with the amount of 15～30 weight parts.
Then, slurry or the paste that as above obtains is shaped to desired shape.Here, specifically, can come moulding by molding modes such as extrusion moulding, injection molding method, casting moulding, scraper plate methods.Then,, burn till again, make aluminum nitride sintered product the degreasing of gained formed body.Above-mentioned moulding also can be carried out granulation with above-mentioned slurry or paste by spray-drier, then prilling powder is carried out mould molding, for example can pass through the moulding of isostatic cool pressing method.In addition, degreasing is preferably carried out under 450～650 ℃ in air, burns till preferably and carries out under 1700～1900 ℃ in nitrogen atmosphere.
In addition, can not use organic binder bond, but come moulding by the compressed moulding method.For example, can be manufactured in single screw rod shaper the preformed base substrate of mixed powder (green body) with aluminium nitride powder and sintering aid powder, with this base substrate in CIP (isostatic cool pressing) shaper with 1～4t/cm
2Extrusion forming, thereby preparation formed body.In this case, do not need degreasing process, preferred under these conditions the formed body of gained is burnt till, make aluminum nitride sintered product.
In addition, above-mentioned aluminum nitride sintered product become on the surface on junction surface form alumina layer before, can on this surface, implement processing such as roughened, milled processed.As roughened, can enumerate the etching that utilizes alkaline aqueous solution, sandblast etc.In addition, as milled processed, can enumerate the grinding of using abrasive particle, online electrolytic dressing grinding etc.
Then, on the surface that becomes the junction surface of gained aluminum nitride sintered product, form alumina layer, for example, form by following oxide treatment.That is to say, aluminum nitride sintered product is heated in oxygenous atmosphere, form alumina layer from the teeth outwards.
As oxygenous gas, air is the easiest, but can use purity oxygen, with rare gas element (for example the oxygen that in rare gas elementes such as nitrogen, carbonic acid gas, argon gas, dilutes etc.) and/or air with the gas of oxygen dilution etc.Oxygen concentration in the oxygenous gas is preferably more than 20%.
The dew point of oxygenous gas is preferably below-25 ℃, more preferably-40 ℃～-30 ℃.In order to make dew point in above-mentioned scope, it is dry in advance with employed gas to pass through suitable means such as compression, siccative drying.
Heating temperature is generally 1100～1300 ℃, is preferably 1130～1270 ℃, is generally 1～100 hour heat-up time, is preferably 5～30 hours.
By this oxide treatment, the aluminium nitride on aluminum nitride sintered product surface is oxidized, generates α-Al
2O
3, on the surface that becomes the junction surface of aluminum nitride sintered product, form alumina layer.Along with this α-Al
2O
3Generation, the weight of aluminum nitride sintered product increases, so the increasing amount of the weight that causes of oxidation becomes the yardstick of alumina layer thickness.1.6～6.5mg/m
2The increase of weight be equivalent to 2～10 μ m.
In addition, in order to form finer and close alumina layer, can adopt the method for putting down in writing in the TOHKEMY 2005-159334 communique.That is to say, can adopt the method that comprises following operation: in intensification, do not make oxygen solid solution ground that aluminum nitride sintered product is not heated to operation (this operation abbreviates " heating process " as) than the temperature more than the temperature of low 300 ℃ of the oxidation onset temperature of aluminum nitride sintered product basically, and the required surface that is heated in this operation than the aluminum nitride sintered product more than the temperature of low 300 ℃ of the oxidation onset temperature of aluminum nitride sintered product is contacted with oxygen, remain on the temperature higher then than the oxidation onset temperature of aluminum nitride sintered product, with the surface oxidation of aluminum nitride sintered product, thus the operation (this operation abbreviates " oxidation operation " as) of formation alumina layer.
Here, oxidation onset temperature under atmospheric pressure is 1100 ℃.In addition, from obtaining the viewpoint of good alumina layer, the temperature that beginning contacts with oxygen it is desirable to more than the oxidation onset temperature.
In addition, alumina layer 103 can be by θ-Al
2O
3The layer that constitutes.Forming by θ-Al
2O
3During the layer that constitutes, preferably use the method for putting down in writing in the TOHKEMY 2001-294492 communique.Specifically, aluminum nitride sintered product under steam partial pressure is oxygen atmosphere below the 1.0kPa, when handling 0.5～30 hour under 800～1000 ℃ temperature, is formed by θ-Al
2O
3The layer that constitutes.
In addition, though figure 1 illustrates the situation that only on junction surface 102, forms alumina layer 103, also can on the surface beyond the junction surface 102 of aluminum nitride sintered product 101, form alumina layer.That is to say, in aluminum nitride sintered product 101, on junction surface 102, form alumina layer 103 at least and get final product.In addition, in order only on junction surface 102, to form alumina layer 103, can use known method.
Next, as shown in Figure 2, in aluminum nitride sintered product 101, on the junction surface 102 that is formed with alumina layer 103, form the paste layer 201 that comprises alkaline earth metal compound.
Aforesaid paste comprises alkaline earth metal compound, preferred package alkaline including earth metal salt, oxide compound.
As alkaline earth salt, can enumerate calcium salts such as lime carbonate, nitrocalcite.In the middle of these, lime carbonate is preferred.As alkaline earth metal oxide, can enumerate calcium oxide, CaOAl
2O
3, 3CaOAl
2O
3Deng.These alkaline earth metal compounds can use separately also and can be use mixing two or more.
In addition, from the viewpoint that begins at low temperatures to react, aforesaid paste can further contain aluminum oxide, and with respect to 100 weight part alkaline earth metal compounds, usually with 40～250 weight parts, preferably containing aluminum oxide with the amount of 50～200 weight parts is ideal.
As aluminum oxide, the fines that particle diameter is little is preferred.
Aforesaid paste can further contain solvent, dispersion agent etc.
As solvent, can enumerate terpinol etc.Per 100 weight part alkaline earth metal compound powder, this solvent preferably use with the amount of 30～80 weight parts usually with 10～90 weight parts.In addition, when containing alkaline earth metal compound and aluminum oxide, be the alkaline earth metal compound and the aluminum oxide of 100 weight parts with respect to total amount, solvent preferably uses with the amount of 30～80 weight parts usually with 10～90 weight parts.Solvent can use separately also and can be use mixing two or more.
As dispersion agent, can enumerate ethyl cellulose etc.Per 100 weight part alkaline earth metal compound powder, this dispersion agent preferably use with the amount of 1～10 weight part usually with 0.5～20 weight part.Dispersion agent can use separately also and can be use mixing two or more.
In alkaline earth metal compound, add mentioned component as required and these are mixed and obtain aforesaid paste.
As the method that on junction surface 102, forms the layer that constitutes by aforesaid paste, can enumerate coating, silk screen printing etc.
The thickness of paste layer 201 is preferably 10～1000 μ m, and more preferably 50～500 μ m are ideal.
Then, as shown in Figure 3, with the junction surface that is formed with alumina layer 303 302 of aluminum nitride sintered product 301 attached on the paste layer 201.That is to say that the mode that contacts with paste layer 201 according to the junction surface that is formed with alumina layer 303 302 of aluminum nitride sintered product 301 is provided with aluminum nitride sintered product 301.In addition, the aluminum nitride sintered product 301 that is formed with alumina layer 303 on junction surface 302 can use the sintered compact identical with aluminum nitride sintered product 101.
At last, heat treated is carried out attached to after on the paste layer 201 in junction surface 302.That is to say, be in above-mentioned junction surface (102,302) relatively and under the state that has paste layer 201 between above-mentioned junction surface (102,302), carry out heat treated at two the above-mentioned aluminum nitride sintered products (101,301) that are formed with alumina layer on junction surface (102,302).
Heating temperature is preferably 1200～1700 ℃, more preferably 1300～1650 ℃.Like this, manufacturing method according to the invention owing on the junction surface of aluminum nitride sintered product alumina layer is set, can obtain the conjugant of firm engagement by heating at a lower temperature.In addition, owing to engage at a lower temperature, the conjugant of gained is not found the distortion of aluminum nitride sintered product part.
As the atmosphere of heating, can enumerate argon gas atmosphere, nitrogen atmosphere etc.From using the viewpoint of aluminum nitride sintered product, nitrogen atmosphere is preferred.
In addition, because the junction surface of aluminum nitride sintered product is provided with alumina layer, even heating under atmospheric pressure also can engage aluminum nitride sintered product the resistance to air loss height at the junction surface of gained each other securely.In addition, the distortion of the aluminum nitride sintered product part that produces under the situation that the gained conjugant can also suppress evenly not exert pressure owing to the condition of exerting pressure.In addition, under the situation of using hot-pressed sintering furnace etc. to heat and exerting pressure, the joint of the sintered compact of big sintered compact (for example more than the φ 500mm), complicated shape has difficulty, and in manufacture method of the present invention, has the advantage that can easily this sintered compact be engaged with each other.
In addition, in manufacture method of the present invention, heating under atmospheric pressure obtains conjugant, also can heat to obtain conjugant under the pressure of for example 0.1MPa～300MPa.
Be preferably 1～30 hour heat-up time, more preferably 3～10 hours.
As the device that is used to heat, can enumerate normal pressure-sintered stove, hot-pressed sintering furnace, hot isostatic pressing stove.
Like this, manufacturing method according to the invention obtains aluminum nitride bonded body, in the present invention, can only on the junction surface 102 of aluminum nitride sintered product 101, form paste layer 201 as mentioned above, yet also can on the junction surface 302 of the junction surface 102 of aluminum nitride sintered product 101 and aluminum nitride sintered product 301, all form the paste layer, two paste layers are adhered to, carry out heat treated.
In addition, after forming paste layer 201, can paste layer 201 is dry under the temperature of room temperature～80 ℃, adhere to the junction surface that is formed with alumina layer 303 302 of aluminum nitride sintered product 301 then.
As shown in Figure 4, in the aluminum nitride bonded body 400 that obtains as mentioned above, do not see alumina layer on the junction surface 401, aluminum nitride sintered product engages each other securely, and in addition, this conjugant has high resistance to air loss.In addition, in Fig. 4, schematically show the junction surface, but, therefore do not observe joint interface usually by the SEM photo because the actual conjugant that obtains engages securely.This is considered to owing to produced following phenomenon in above-mentioned joint operation.For example, contain lime carbonate (CaCO in use
3) the situation of paste as aforesaid paste under, by the heating, lime carbonate (CaCO
3) at first form calcium oxide (CaO).Then, calcium oxide (CaO) and the aluminum oxide (Al that is present in the aluminum nitride sintered product surface
2O
3) reaction, generate CaOAl
2O
3, CaO2Al
2O
3Deng calcium aluminate, this calcium aluminate is diffused in the aluminum nitride sintered product piece along crystal boundary.Therefore, think and do not have alumina layer on the junction surface 401.
Contain in the situation of paste of calcium oxide (CaO) in use also identical, by heating, this calcium oxide (CaO) and the aluminum oxide (Al that is present in the aluminum nitride sintered product surface
2O
3) reaction, generate aforesaid calcium aluminate layer.In addition, contain in use under the situation of paste of calcium oxide (CaO) and aluminum oxide, by heating, contained aluminum oxide and be present in the aluminum oxide (Al on aluminum nitride sintered product surface in this calcium oxide (CaO) and the paste
2O
3) reaction, generate aforesaid calcium aluminate.And then think, contain CaOAl in use
2O
3, 3CaOAl
2O
3Deng the situation of paste under, by heating, generated above-mentioned calcium aluminate equally.Think that any situation in the middle of these all is because the calcium aluminate that is generated is diffused in the aluminum nitride sintered product piece along crystal boundary, therefore finally obtains the conjugant of oxygen-free aluminium lamination on the junction surface.
In addition, in the present invention, think that heating at a lower temperature can be with the reasons are as follows that aluminum nitride sintered product engages each other securely.
The reaction that with the calcium oxide is the alkaline earth metal compound of representative and aluminum oxide takes place since about 1400 ℃ lesser temps.Think that the middle mutually solid solution of the calcium aluminate that reaction is generated when further heating up has the AlN that comes from aluminum nitride particle.CaO-Al by such generation
2O
3-AlN, AlN can engage each other securely.The AlN of solid solution separates out in process of cooling again in liquid phase.CaO-Al
2O
3Liquid composition be diffused in the aluminum nitride sintered product along crystal boundary, become in the junction surface and can't see.
Because the aluminum nitride bonded body 400 of Huo Deing is that heating is made under lower temperature as mentioned above, the energy of deformation of junction surface 401 and aluminum nitride sintered product part (101,301) accesses inhibition.
Followingly further specifically describe the present invention according to embodiment, yet, the invention is not restricted to these embodiment.
[embodiment]
1. evaluation method
1) evaluation of joint interface
Use secondary electron scanning electron microscope (SEM), observe the aluminum nitride sintered product joint interface.
2) bond strength
Room temperature bend test method (JIS C2141) according to fine ceramics carries out 3 pliability tests.Length of support is from being set at 30mm.During aluminium nitride after estimate engaging, the be engaged with each other conjugant 700 that obtained of the aluminum nitride bonded body 702 of 30mm * 30mm, thickness 3mm is processed into the test film 703 (with reference to Fig. 7) of total length 40mm, thickness 3mm.That is to say, along the dotted line cut-out of Fig. 7.Then, dispose this test film 703, make junction surface 701 be positioned at the center between fulcrum, apply load-carrying from the top at this junction surface 701.
3) gas-tightness test
In order to estimate the degree of engagement of joint interface, the aluminum nitride sintered product that use will be processed into the hollow cylindrical of φ 50mm, height 30mm, thickness 8mm engages the conjugant that forms with the aluminum nitride sintered product of the plectane that is processed into φ 50mm, thickness 5mm, by ULVAC, the helium leak detector (model HELIOT 704D2) that Inc. makes carries out helium and visits the leakage test.
2. on the junction surface, be formed with the aluminum nitride sintered product of alumina layer
1) on the junction surface, is formed with the aluminum nitride sintered product (A-1-1)～(A-1-3) of alumina layer
(moral mountain company makes, SH-15) in oxygen atmosphere, carry out oxide treatment under 1200 ℃, 5 hours condition with the aluminum nitride sintered product of 30mm * 30mm, thickness 3mm.Acquisition is formed with the aluminum nitride sintered product (A-1-1) (the following aluminum nitride sintered product (A-1-1) that only is called) of the alumina layer of 2 μ m thickness on the surface of all faces that comprise the junction surface.
To being processed into φ 50mm, the highly aluminum nitride sintered product of the hollow cylindrical of 30mm, thickness 8mm (moral mountain company manufacturing, SH-15) and be processed into the aluminum nitride sintered product of the plectane of φ 50mm, thickness 5mm (moral mountain company makes, SH-15) carry out same oxide treatment, obtained on the surface of all faces that comprise the junction surface, to be formed with aluminum nitride sintered product (A-1-2) and (A-1-3) (following aluminum nitride sintered product (A-1-2), (A-1-3) of only being called respectively) of the alumina layer of 2 μ m thickness respectively.
2) be formed with the aluminum nitride sintered product (A-2-1)～(A-2-3) of alumina layer on the junction surface
(moral mountain company makes, SH-15) in oxygen atmosphere, carry out oxide treatment under 1200 ℃, 30 hours condition with the aluminum nitride sintered product of 30mm * 30mm, thickness 3mm.Acquisition is formed with the aluminum nitride sintered product (A-2-1) (the following aluminum nitride sintered product (A-2-1) that only is called) of the alumina layer of 5 μ m thickness on the surface of all faces that comprise the junction surface.
To being processed into φ 50mm, the highly aluminum nitride sintered product of the hollow cylindrical of 30mm, thickness 8mm (moral mountain company manufacturing, SH-15) and be processed into the aluminum nitride sintered product of the plectane of φ 50mm, thickness 5mm (moral mountain company makes, SH-15) carry out same oxide treatment, obtained on the surface of all faces that comprise the junction surface, to be formed with aluminum nitride sintered product (A-2-2) and (A-2-3) (following aluminum nitride sintered product (A-2-2), (A-2-3) of only being called respectively) of the alumina layer of 5 μ m thickness respectively.
3) be formed with the aluminum nitride sintered product (B-1-1)～(B-1-3) of alumina layer on the junction surface
(moral mountain company makes, SH-50) in oxygen atmosphere, carry out oxide treatment under 1200 ℃, 5 hours condition with the aluminum nitride sintered product of 30mm * 30mm, thickness 3mm.Acquisition is formed with the aluminum nitride sintered product (B-1-1) (the following aluminum nitride sintered product (B-1-1) that only is called) of the alumina layer of 2 μ m thickness on the surface of all faces that comprise the junction surface.
To being processed into φ 50mm, the highly aluminum nitride sintered product of the hollow cylindrical of 30mm, thickness 8mm (moral mountain company manufacturing, SH-50) and be processed into the aluminum nitride sintered product of the plectane of φ 50mm, thickness 5mm (moral mountain company makes, SH-50) carry out same oxide treatment, obtained on the surface of all faces that comprise the junction surface, to be formed with aluminum nitride sintered product (B-1-2) and (B-1-3) (following aluminum nitride sintered product (B-1-2), (B-1-3) of only being called respectively) of the alumina layer of 2 μ m thickness respectively.
4) be formed with the aluminum nitride sintered product (A-3-1)～(A-3-3) of alumina layer on the junction surface
(moral mountain company makes, SH-15) in oxygen atmosphere, carry out oxide treatment under 1100 ℃, 2 hours condition with the aluminum nitride sintered product of 30mm * 30mm, thickness 3mm.Acquisition is formed with the aluminum nitride sintered product (A-3-1) (the following aluminum nitride sintered product (A-3-1) that only is called) of the alumina layer of 0.5 μ m thickness on the surface of all faces that comprise the junction surface.
To being processed into φ 50mm, the highly aluminum nitride sintered product of the hollow cylindrical of 30mm, thickness 8mm (moral mountain company manufacturing, SH-15) and be processed into the aluminum nitride sintered product of the plectane of φ 50mm, thickness 5mm (moral mountain company makes, SH-15) carry out same oxide treatment, obtained on the surface of all faces that comprise the junction surface, to be formed with aluminum nitride sintered product (A-3-2) and (A-3-3) (following aluminum nitride sintered product (A-3-2), (A-3-3) of only being called respectively) of the alumina layer of 0.5 μ m thickness respectively.
5) be formed with the aluminum nitride sintered product (A-4-1)～(A-4-3) of alumina layer on the junction surface
(moral mountain company makes, SH-15) in oxygen atmosphere, carry out oxide treatment under 1300 ℃, 15 hours condition with the aluminum nitride sintered product of 30mm * 30mm, thickness 3mm.Acquisition is formed with the aluminum nitride sintered product (A-4-1) (the following aluminum nitride sintered product (A-4-1) that only is called) of the alumina layer of 7 μ m thickness on the surface of all faces that comprise the junction surface.
To being processed into φ 50mm, the highly aluminum nitride sintered product of the hollow cylindrical of 30mm, thickness 8mm (moral mountain company manufacturing, SH-15) and be processed into the aluminum nitride sintered product of the plectane of φ 50mm, thickness 5mm (moral mountain company makes, SH-15) carry out same oxide treatment, obtained on the surface of all faces that comprise the junction surface, to be formed with aluminum nitride sintered product (A-4-2) and (A-4-3) (following aluminum nitride sintered product (A-4-2), (A-4-3) of only being called respectively) of the alumina layer of 7 μ m thickness respectively.
3. engage the preparation of paste
1) engages paste (A)
With ball mill 50g lime carbonate (making with the pure medicine of light company), 50g alumina powder (clear and electrician makes), 60g are mixed as the ethyl cellulose of dispersion agent as the terpinol and the 3g of solvent, preparation engages paste (A).
2) engage paste (B)
With ball mill 100g lime carbonate (making with the pure medicine of light company), 60g are mixed as the ethyl cellulose of dispersion agent as terpinol, the 3g of solvent, preparation engages paste (B).
3) engage paste (C)
With ball mill with 100g 3CaOAl
2O
3, 60g mixes as the ethyl cellulose of dispersion agent as the terpinol of solvent, 3g, preparation engages paste (C).
4) engage paste (D)
With ball mill 100g calcium oxide (making with the pure medicine of light company), 60g are mixed as the ethyl cellulose of dispersion agent as terpinol, the 3g of solvent, preparation engages paste (D).
[embodiment 1-1]
Go up the joint paste (A) that is coated with 300 μ m thickness at aluminum nitride sintered product (A-1-1), configuration another aluminum nitride sintered product (A-1-1) (with reference to Fig. 8 and 9) on joint paste (A) layer that is coated with.This aluminum nitride sintered product (A-1-1) (being in the state that disposes another aluminum nitride sintered product (A-1-1)) is implemented drying treatment in remaining 80 ℃ thermostatic drier.Then, it is configured in the anchor clamps of boron nitride system, heating is 5 hours in nitrogen atmosphere, under 1600 ℃, and (A-1-1) is engaged with each other with aluminum nitride sintered product.The SEM photo of gained conjugant is shown in Figure 6, is bonded into the degree that can not tell the interface.In addition, the result who carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (340MPa) of degree.
[embodiment 1-2]
Go up the joint paste (A) that is coated with 300 μ m thickness at aluminum nitride sintered product (A-1-2), configuration aluminum nitride sintered product (A-1-3) (with reference to Figure 10 and 11) on joint paste (A) layer that is coated with.This aluminum nitride sintered product (A-1-2) (being in the state that disposes aluminum nitride sintered product (A-1-3)) carries out drying treatment in remaining 80 ℃ thermostatic drier.Then, with the same condition of embodiment 1-1 under heat, with the two joint.
The gained conjugant is carried out helium visit the leakage test, leak volume is 5.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 2-1]
Except using aluminum nitride sintered product (B-1-1) to replace the aluminum nitride sintered product (A-1-1), use with the same method of embodiment 1-1 to engage.The result that the conjugant of gained carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (300MPa) of degree.
[embodiment 2-2]
Except use aluminum nitride sintered product (B-1-2) and (B-1-3) replacement aluminum nitride sintered product (A-1-2) and (A-1-3), use with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 5.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 3-1]
Except using aluminum nitride sintered product (A-2-1) to replace the aluminum nitride sintered product (A-1-1), use with the same method of embodiment 1-1 to engage.The result that this conjugant carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (350MPa) of degree.
[embodiment 3-2]
Except use aluminum nitride sintered product (A-2-2) and (A-2-3) replacement aluminum nitride sintered product (A-1-2) and (A-1-3), use with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 5.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 4-1]
Replacing engaging the paste (A) except use engaging paste (B), using with the same method of embodiment 1-1 to engage.The result that this conjugant carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (330MPa) of degree.
[embodiment 4-2]
Replacing engaging the paste (A) except use engaging paste (B), using with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 5.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 5-1]
Replacing engaging the paste (A) except use engaging paste (C), using with the same method of embodiment 1-1 to engage.The result that this conjugant carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (330MPa) of degree.
[embodiment 5-2]
Replacing engaging the paste (A) except use engaging paste (C), using with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 5.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 6-1]
Replacing engaging the paste (A) except use engaging paste (D), using with the same method of embodiment 1-1 to engage.The result that this conjugant carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (360MPa) of degree.
[embodiment 6-2]
Replacing engaging the paste (A) except use engaging paste (D), using with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 5.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 7-1]
Except using aluminum nitride sintered product (A-3-1) to replace the aluminum nitride sintered product (A-1-1), use with the same method of embodiment 1-1 to engage.The result that this conjugant carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (320MPa) of degree.
[embodiment 7-2]
Except use aluminum nitride sintered product (A-3-2) and (A-3-3) replacement aluminum nitride sintered product (A-1-2) and (A-1-3), use with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 8.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
[embodiment 8-1]
Except using aluminum nitride sintered product (A-4-1) to replace the aluminum nitride sintered product (A-1-1), use with the same method of embodiment 1-1 to engage.The result that this conjugant carries out bending strength test shown and engage before aluminum nitride sintered product with the intensity (310MPa) of degree.
[embodiment 8-2]
Except use aluminum nitride sintered product (A-4-2) and (A-4-3) replacement aluminum nitride sintered product (A-1-2) and (A-1-3), use with the same method of embodiment 1-2 to engage.
The gained conjugant is carried out helium visit the leakage test, leak volume is 8.0 * 10
-9Below the atmcc/sec, shown high resistance to air loss.
Claims (3)
1. the manufacture method of an aluminum nitride bonded body, the manufacture method of the aluminum nitride bonded body that it forms for aluminum nitride sintered product is engaged with each other, it is characterized in that, comprise following joint operation: be in aforementioned junction surface relatively and exist between the aforementioned junction surface under the state of the paste layer that comprises alkaline earth metal compound at two aforementioned aluminum nitride sintered products that are formed with alumina layer on the junction surface, under 1300～1700 ℃ temperature, heat, aforementioned aluminum nitride sintered product is engaged with each other.
2. the manufacture method of aluminum nitride bonded body according to claim 1, it is characterized in that, aforementioned joint operation is to form the paste layer that comprises alkaline earth metal compound on the junction surface that is formed with alumina layer of an aforementioned aluminum nitride sintered product, and with the junction surface that is formed with alumina layer of another aforementioned aluminum nitride sintered product attached on this paste layer, under 1300～1700 ℃ temperature, heat the operation that aforementioned aluminum nitride sintered product is engaged with each other then.
3. the manufacture method of aluminum nitride bonded body according to claim 1 and 2, wherein, the thickness of formed alumina layer is 0.1～10 μ m on the junction surface of aforementioned aluminum nitride sintered product.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP318798/2006 | 2006-11-27 | ||
| JP2006318798 | 2006-11-27 |
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|---|---|
| CN101528638A true CN101528638A (en) | 2009-09-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007800397781A Pending CN101528638A (en) | 2006-11-27 | 2007-11-26 | Process for producing aluminum nitride joint product |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP5302689B2 (en) |
| KR (1) | KR101137917B1 (en) |
| CN (1) | CN101528638A (en) |
| TW (1) | TW200823166A (en) |
| WO (1) | WO2008065980A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3406583B1 (en) * | 2016-02-26 | 2021-07-14 | Kyocera Corporation | Ceramic bonded body |
| JP6867907B2 (en) * | 2017-07-31 | 2021-05-12 | 日本特殊陶業株式会社 | Ceramic joints and methods for manufacturing ceramic joints |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0725617B2 (en) * | 1985-08-22 | 1995-03-22 | 住友電気工業株式会社 | Aluminum nitride substrate and manufacturing method thereof |
| JP3604888B2 (en) * | 1997-01-30 | 2004-12-22 | 日本碍子株式会社 | Jointed body of aluminum nitride-based ceramics substrate, method of manufacturing jointed body of aluminum nitride-based ceramics base, and bonding agent |
| JP4077427B2 (en) * | 1997-01-30 | 2008-04-16 | 日本碍子株式会社 | Bonded body of aluminum nitride ceramic base material and manufacturing method thereof |
| JPH10154770A (en) * | 1997-12-08 | 1998-06-09 | Toshiba Corp | Manufacture of ceramic package |
| JPH11343178A (en) * | 1998-06-02 | 1999-12-14 | Fuji Electric Co Ltd | Bonding of copper plate and non-oxidized ceramics |
| JP4787568B2 (en) * | 2004-11-16 | 2011-10-05 | 日本碍子株式会社 | Bonding agent, aluminum nitride bonded body, and manufacturing method thereof |
-
2007
- 2007-11-19 TW TW096143688A patent/TW200823166A/en unknown
- 2007-11-26 JP JP2008546972A patent/JP5302689B2/en not_active Expired - Fee Related
- 2007-11-26 KR KR1020097008605A patent/KR101137917B1/en not_active IP Right Cessation
- 2007-11-26 CN CNA2007800397781A patent/CN101528638A/en active Pending
- 2007-11-26 WO PCT/JP2007/072726 patent/WO2008065980A1/en active Application Filing
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| Publication number | Publication date |
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| TW200823166A (en) | 2008-06-01 |
| KR20090084831A (en) | 2009-08-05 |
| WO2008065980A1 (en) | 2008-06-05 |
| KR101137917B1 (en) | 2012-05-09 |
| JP5302689B2 (en) | 2013-10-02 |
| JPWO2008065980A1 (en) | 2010-03-04 |
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