JPH0440314B2 - - Google Patents
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- Publication number
- JPH0440314B2 JPH0440314B2 JP19829687A JP19829687A JPH0440314B2 JP H0440314 B2 JPH0440314 B2 JP H0440314B2 JP 19829687 A JP19829687 A JP 19829687A JP 19829687 A JP19829687 A JP 19829687A JP H0440314 B2 JPH0440314 B2 JP H0440314B2
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- silicon nitride
- sintering
- weight
- sin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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- 239000000843 powder Substances 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 12
- 238000005304 joining Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims 1
- 230000000996 additive effect Effects 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910017945 Cu—Ti Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、窒化ケイ素セラミツクスを接合する
接合方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a joining method for joining silicon nitride ceramics.
従来の窒化ケイ素セラミツクスの接合方法に
は、次のような三つの方法がある。
There are three conventional methods for bonding silicon nitride ceramics:
(1) 窒化ケイ素（Si3N4）粉末を被接合体間に挟
んで加圧加熱する。(1) Silicon nitride (Si 3 N 4 ) powder is sandwiched between objects to be joined and heated under pressure.
(2) 酸化物系のガラス粉末を被接合体間に挾んで
加熱する。(2) Sandwich oxide glass powder between objects to be joined and heat.
(3) Cu−Ti，Al等の金属箔を被接合体間に挾ん
で加熱する。(3) A metal foil such as Cu-Ti or Al is sandwiched between the objects to be joined and heated.
上記(1)の方法は、Si3N4の焼結と類似したメカ
ニズムを利用しており、サブミクロンオーダーの
焼結性のよいSi3N4微粉末を被接合体間に挾み、
通常の焼結条件（1800℃，20MPa（メガ・パスカ
ル））でホツトプレス処理することによつて接合
される。 The method (1) above uses a mechanism similar to the sintering of Si 3 N 4 , in which submicron-order Si 3 N 4 fine powder with good sinterability is sandwiched between the objects to be joined.
They are joined by hot pressing under normal sintering conditions (1800℃, 20MPa (mega Pascal)).
(2)の方法は、1500℃前後に融点を持つ酸化物系
（例えばCaO−SiO2）ガラス粉末を被接合体間に
挾み、液相を生成する温度まで加熱することによ
つて接合される。 In method (2), oxide-based (e.g. CaO-SiO 2 ) glass powder with a melting point around 1500°C is sandwiched between the objects to be joined and heated to a temperature that generates a liquid phase. Ru.
(3)の方法は、窒素との親和力が強いTi，Al等
の元素を含む1000℃前後の低融点のろう材を被接
合体間に挾み、液相を生成する温度まで加熱する
ことによつて接合される。なお、一般に接合層
は、TiNやAlNの他にシリサイドや単体金属を
含んでいる。 Method (3) involves sandwiching a brazing filler metal with a low melting point of around 1000℃ between the objects to be joined, which contains elements such as Ti and Al that have a strong affinity with nitrogen, and heating it to a temperature that generates a liquid phase. It is then joined. Note that the bonding layer generally contains silicide or a single metal in addition to TiN or AlN.
上記した従来技術の(1)の方法においては、窒化
ケイ素セラミツクス母材に匹敵する強度と耐熱性
を有するものの、通常の焼結条件と同程度の温度
及び圧力で処理しなければならず、従つて母材の
変形等が生じ易く、接合によつて大型部材を製造
することの利点が失われるという問題点もあつ
た。
Although the method (1) of the prior art described above has strength and heat resistance comparable to that of silicon nitride ceramic base material, it must be processed under the same temperature and pressure as normal sintering conditions. There was also a problem in that the base material was easily deformed and the advantages of manufacturing large members by joining were lost.
また(2)及び(3)の方法においては、何れも、比較
的低温低圧下の処理で接合できるものの、(2)の方
法においてはガラス相、また(3)の方法においては
金属相をそれぞれ接合層に含むために、強度、耐
熱性とも母材よりも劣るという問題点があつた。 In addition, although methods (2) and (3) can both be bonded by processing at relatively low temperature and low pressure, method (2) has a glass phase, and method (3) has a metal phase, respectively. Since it is included in the bonding layer, it has a problem in that it is inferior to the base material in both strength and heat resistance.
本発明は、母材に匹敵する強度と耐熱性とを有
す窒化ケイ素セラミツクス接合体を、低温低圧下
の処理で作製する方法を提供することを技術的課
題としている。 The technical object of the present invention is to provide a method for producing a silicon nitride ceramic bonded body having strength and heat resistance comparable to that of the base material by processing at low temperature and low pressure.
上記した従来技術の問題点及び技術的課題を解
決するために、本発明は、被接合体間に、酸素含
有量が１重量％以上15重量％以下で、粒径がサブ
ミクロンオーダー以下であるSiNxOy微粉末に、
窒化ケイ素セラミツクスの焼結に通常用いられる
Al2O3，MgO，Y2O3等の焼結助剤微粉末１種類
以上を０重量％又はそれ以上の割合で添加混合し
たものを挾んで加熱することを特徴とする窒化ケ
イ素セラミツクスの接合方法を用いる。
In order to solve the problems and technical problems of the prior art described above, the present invention provides that the oxygen content between the objects to be joined is 1% by weight or more and 15% by weight or less, and the particle size is on the submicron order or less. SiN x O y fine powder,
Usually used for sintering silicon nitride ceramics
Silicon nitride ceramics is produced by heating a mixture of one or more sintering aid fine powders such as Al 2 O 3 , MgO, Y 2 O 3 in a proportion of 0% by weight or more. Use a joining method.
本発明は、基本的には液相焼結と類似したメカ
ニズムを利用している。即ち、窒化ケイ素母材中
に含まれる焼結助剤成分が拡散して、SiNxOy微
粒子表面上に形成されているSiO2との間で液相
を生成することによつて、焼結が進行し、接合が
行われる。この場合、低温で焼結するために粒径
は小さい方が望ましく、サブミクロンオーダー以
下であることが必要である。また、SiNxOy微粉
末の酸素含有量が１重量％以下の時には低温で液
相が生成せず、15重量％以上の時には、酸化物相
の強度、耐熱性が支配的になり好ましくない。
The present invention basically utilizes a mechanism similar to liquid phase sintering. In other words, the sintering aid component contained in the silicon nitride base material diffuses and forms a liquid phase with SiO 2 formed on the surface of the SiN x O y fine particles, thereby promoting sintering. progresses and joining is performed. In this case, in order to perform sintering at a low temperature, the particle size is preferably small, and needs to be on the submicron order or less. In addition, when the oxygen content of the SiN x O y fine powder is less than 1% by weight, no liquid phase is generated at low temperatures, and when it is more than 15% by weight, the strength and heat resistance of the oxide phase become dominant, which is undesirable. .
一般に、低温では液相を生成する組成域が狭
く、SiNxOy微粉末中の酸素量に敏感となり、
SiNxOy微粉末作製上不都合であるため、予め焼
結助剤成分を微粉末の状態で混合しておくとよ
い。この際に、接合時の熱処置条件に応じて、液
相を生成する許容酸素量の幅が最も広がるように
添加する焼結助剤微粉末の種類と量を選択するの
が望ましい。 Generally, at low temperatures, the composition range that produces a liquid phase is narrow, and it becomes sensitive to the amount of oxygen in the SiN x O y fine powder.
Since this is inconvenient in preparing SiN x O y fine powder, it is preferable to mix the sintering aid component in the form of fine powder in advance. At this time, it is desirable to select the type and amount of the sintering aid fine powder to be added so as to widen the range of the permissible amount of oxygen for forming a liquid phase, depending on the heat treatment conditions during bonding.
次に、本発明の接合方法を実施した実施例につ
いて説明する。
Next, an example in which the joining method of the present invention is implemented will be described.
この実施例では、Al2O3，MgOを焼結助剤とし
た常圧焼結品である15mmφ（直径）×30mm（長
さ）の窒化ケイ素セラミツクスの被接合面に、
SiNxOy微粉末にAl2O3焼結助剤微粉末を０及び３
重量％添加混合しアセトンに分散したものを塗布
し、乾燥させたものを重ね合せて、１気圧のN2
雰囲気中でホツトプレス処理した。処理条件は
1500℃，15MPa，30分である。 In this example, on the surface to be joined of silicon nitride ceramics of 15 mmφ (diameter) x 30 mm (length), which is a pressureless sintered product using Al 2 O 3 and MgO as sintering aids,
SiN x O y fine powder and Al 2 O 3 sintering aid fine powder 0 and 3
After adding and mixing % by weight and dispersing it in acetone, apply it, dry it, stack it on top of each other, and apply 1 atm of N 2
Hot press treatment was carried out in an atmosphere. The processing conditions are
1500℃, 15MPa, 30 minutes.
上記SiNxOy微粉末は、NH3雰囲気中でSiを蒸
発させる反応性ガス中蒸発法によつて作製した。
平均粒径は0.05μｍである。 The SiN x O y fine powder was produced by a reactive gas evaporation method in which Si is evaporated in an NH 3 atmosphere.
The average particle size is 0.05 μm.
また、Al2O3焼結助剤微粉末は、O2雰囲気中で
Alを蒸発させる反応性ガス中蒸発法によつて作
製した。平均粒径は0.05μｍである。 In addition, Al 2 O 3 sintering aid fine powder can be used in O 2 atmosphere.
It was fabricated using a reactive gas evaporation method to evaporate Al. The average particle size is 0.05 μm.
次に、上記実施例の作用を、第１図及び第２図
で説明する。 Next, the operation of the above embodiment will be explained with reference to FIGS. 1 and 2.
第１図は、Al2O3焼結助剤微粉末が０重量％、
つまり該微粉末を添加しない時のSiNxOy微粉末
中の酸素量と接合強度との関係を示す線図であ
る。 Figure 1 shows that the Al 2 O 3 sintering aid fine powder is 0% by weight;
In other words, it is a diagram showing the relationship between the amount of oxygen in the SiN x O y fine powder and the bonding strength when the fine powder is not added.
図中、斜線を施こした部分ａ、即ち酸素量が４
重量％から７重量％まででは、破断が窒化ケイ素
母材中で起こつており、母材強度に匹敵する接合
強度が得られていると考えられる。上記範囲よ
り、酸素量が少ない場合及び多い場合においても
接合はなされたが、強度は急激に低下した。この
実施例による処理条件下においては、母材中から
拡散で供給されるAl2O3及びMgOの量に対して液
相を生成する酸素量（SiO2量に相当）が少ない
ため、図のように許容酸素量幅が狭い挙動を示
す。なお、酸素量が１重量％以下及び15重量％以
上の時には、接合がなされなかつた。 In the figure, the shaded area a, that is, the oxygen amount is 4
From % to 7% by weight, fracture occurs in the silicon nitride base material, and it is considered that a bonding strength comparable to the strength of the base material is obtained. Bonding was achieved even when the amount of oxygen was lower or higher than the above range, but the strength sharply decreased. Under the treatment conditions of this example, the amount of oxygen (equivalent to the amount of SiO 2 ) that generates the liquid phase is small compared to the amount of Al 2 O 3 and MgO supplied by diffusion from the base material, so the As shown, the permissible oxygen amount range is narrow. Note that no bonding was achieved when the oxygen content was 1% by weight or less and 15% by weight or more.
第２図は、Al2O3焼結助剤微粉末を３重量％添
加混合した時のSiNxOy微粉末中の酸素量と接合
強度との関係を示す線図である。 FIG. 2 is a diagram showing the relationship between the amount of oxygen in SiN x O y fine powder and bonding strength when 3% by weight of Al 2 O 3 sintering aid fine powder is added and mixed.
図中、斜線を施こした部分ｂ、即ち酸素量が２
重量％から10重量％まででは、母材内で破断し
た、このように、Al2O3を混合することによつ
て、液相を生成する酸素量（SiO2量）の幅が広
がつたために、図のような挙動を示している。 In the figure, the shaded area b, that is, the amount of oxygen is 2
From wt% to 10 wt%, the amount of oxygen ( SiO2 amount) that breaks in the base metal increases by mixing Al2O3 . Therefore, it exhibits the behavior shown in the figure.
上記した実施例では、処理温度を1500℃とした
が、Al2O3−MgO−SiO2系で液相を生じる温度
（約1400℃）以上であればよい。また、ホツトプ
レス処理する代わりに、予め静水圧等を用いて圧
粉したのち加熱する方法を用いてもよい。 In the above embodiments, the treatment temperature was 1500°C, but it may be any temperature higher than the temperature at which a liquid phase occurs in the Al2O3 - MgO- SiO2 system (approximately 1400°C). Furthermore, instead of hot pressing, a method may be used in which the powder is compacted using hydrostatic pressure or the like in advance and then heated.
また、本発明で用いることのできる窒化ケイ素
セラミツクスとしては、焼結助剤としてAl2O3と
MgOを使用したものに限らず、他の焼結助剤を
用いたものでもよい。この際、接合時の処理条件
及び添加する焼結助剤微粉末の種類と量は、それ
ぞれの系に最適のものを選択しなければならな
い。 In addition, silicon nitride ceramics that can be used in the present invention include Al 2 O 3 and sintering aids.
The material is not limited to the one using MgO, but may be one using other sintering aids. At this time, the processing conditions during bonding and the type and amount of the sintering aid fine powder to be added must be selected optimally for each system.
また、SiNxOy微粉末及びAl2O3焼結助剤微粉末
を反応性ガス中蒸発法によつて作製したが、他の
方法例えばCVD法や湿式法等を用いて作製して
もよい。 In addition, although the SiN x O y fine powder and the Al 2 O 3 sintering aid fine powder were produced by the evaporation method in a reactive gas, they could also be produced using other methods such as the CVD method or the wet method. good.
以上説明したように、本発明によれば、窒化ケ
イ素セラミツクスの被接合体間に、酸素含有量が
１重量％以上15重量％以下で、粒径がサブミクロ
ンオーダー以下であるSiNxOy微粉末を挾んで加
熱するようにしたことにより、粒界に効果的に液
相を生成させることができ、そのため、低温で接
合でき、且つ接合層の主成分はSi3N4であるた
め、母材強度に匹敵する接合強度が得られるとい
う効果を奏する。
As explained above, according to the present invention, SiN By sandwiching the powder and heating it, it is possible to effectively generate a liquid phase at the grain boundaries. Therefore, it is possible to bond at a low temperature, and since the main component of the bonding layer is Si 3 N 4 , it is possible to This has the effect of providing a bonding strength comparable to the strength of the materials.
また、焼結助剤微粉末を混合することにより、
液相を生成する組成域が広がり、そのため、高強
度の接合が得られるSiNxOy微粉末中の酸素量の
範囲がより広くなるという効果を奏する。 In addition, by mixing sintering aid fine powder,
This has the effect of widening the composition range in which a liquid phase is generated, and therefore widening the range of oxygen content in the SiN x O y fine powder that allows high-strength bonding to be obtained.
第１図及び第２図は本発明の一実施例の作用を
示す線図であつて、第１図はAl2O3焼結助剤微粉
末を添加しない時のSiNxOy微粉末中の酸素量と
接合強度との関係を示す線図、第２図はAl2O3焼
結助剤微粉末を３重量％添加した時の第１図と同
様の関係を示す線図である。
ａ，ｂ……破断が窒化ケイ素セラミツクス母材
内で起こつた領域。
FIG. 1 and FIG. 2 are diagrams showing the operation of one embodiment of the present invention, and FIG. 1 is a diagram showing the effect of SiN x O y in fine powder when Al 2 O 3 sintering aid fine powder is not added. Figure 2 is a diagram showing the relationship between the amount of oxygen and bonding strength, and Figure 2 is a diagram showing the same relationship as Figure 1 when 3% by weight of Al 2 O 3 sintering aid fine powder is added. a, b...Regions where fracture occurred within the silicon nitride ceramic matrix.
Claims (1)
重量％以下で、粒径がサブミクロンオーダー以下
であるSiNxOy微粉末に、窒化ケイ素セラミツク
スの焼結に通常用いられる焼結助剤微粉末１種類
以上を０重量％又はそれ以上の割合で添加混合し
たものを挾んで加熱することを特徴とする窒化ケ
イ素セラミツクスの接合方法。 ２ 上記焼結助剤微粉末がAl2O3，MgO，Y2O3
等である特許請求の範囲第１項記載の窒化ケイ素
セラミツクスの接合方法。[Claims] 1. Oxygen content between the objects to be joined is 1% by weight or more15
One or more types of sintering aid fine powder commonly used in sintering silicon nitride ceramics is added to SiN x O y fine powder with a particle size of submicron order or less in a proportion of 0% by weight or more. A method for bonding silicon nitride ceramics, characterized by sandwiching and heating the additive mixture. 2 The sintering aid fine powder is Al 2 O 3 , MgO, Y 2 O 3
A method for joining silicon nitride ceramics according to claim 1, wherein
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19829687A JPS6442369A (en) | 1987-08-10 | 1987-08-10 | Method for joining silicon nitride ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19829687A JPS6442369A (en) | 1987-08-10 | 1987-08-10 | Method for joining silicon nitride ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6442369A JPS6442369A (en) | 1989-02-14 |
| JPH0440314B2 true JPH0440314B2 (en) | 1992-07-02 |
Family
ID=16388768
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19829687A Granted JPS6442369A (en) | 1987-08-10 | 1987-08-10 | Method for joining silicon nitride ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6442369A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4018715A1 (en) * | 1990-06-12 | 1991-12-19 | Bayer Ag | METHOD FOR PRODUCING METAL AND / OR CERAMIC COMPOSITE PARTS |
| DE19604844C2 (en) * | 1996-02-10 | 1998-02-26 | Forschungszentrum Juelich Gmbh | Bonding of non-oxide ceramic, ceramic-metallic or metallic bodies and bodies manufactured according to the method |
| JP5959170B2 (en) * | 2011-09-05 | 2016-08-02 | 三井金属鉱業株式会社 | Ceramic bonded body and manufacturing method thereof |
-
1987
- 1987-08-10 JP JP19829687A patent/JPS6442369A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6442369A (en) | 1989-02-14 |
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