JPH0458431B2 - - Google Patents
Info
- Publication number
- JPH0458431B2 JPH0458431B2 JP6129887A JP6129887A JPH0458431B2 JP H0458431 B2 JPH0458431 B2 JP H0458431B2 JP 6129887 A JP6129887 A JP 6129887A JP 6129887 A JP6129887 A JP 6129887A JP H0458431 B2 JPH0458431 B2 JP H0458431B2
- Authority
- JP
- Japan
- Prior art keywords
- ceramics
- alloy
- metal
- sputtering
- joining
- 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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- 239000000919 ceramic Substances 0.000 claims description 38
- 239000011651 chromium Substances 0.000 claims description 34
- 239000000956 alloy Substances 0.000 claims description 22
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 229910052804 chromium Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 238000004544 sputter deposition Methods 0.000 claims description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 14
- 239000010953 base metal Substances 0.000 claims description 14
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 14
- 238000005304 joining Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 229910018487 Ni—Cr Inorganic materials 0.000 claims 2
- 238000010030 laminating Methods 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000000635 electron micrograph Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000005548 dental material Substances 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910000599 Cr alloy Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000011351 dental ceramic Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910000923 precious metal alloy Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
- Ceramic Products (AREA)
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は歯科用材料あるいはガスタービン用材
料のような耐熱高強度材料などの製造に適用でき
る金属とセラミツクスとの接合方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for joining metal and ceramics that can be applied to the production of heat-resistant, high-strength materials such as dental materials or gas turbine materials.
［従来の技術］
近年セラミツクスのもつ美観や耐熱性と金属の
もつ強度や加工性とを兼備した材料として金属と
セラミツクスとの複合材料が種々開発されてい
る。[Prior Art] In recent years, various composite materials of metal and ceramics have been developed as materials that combine the beauty and heat resistance of ceramics with the strength and workability of metals.
例えば歯科補綴修復物は貴金属合金とセラミツ
クス（陶材）を接合させた審美性のある金属焼付
ポーセレンと称する材料が主流となつている。こ
の場合両者の接合は、貴金属材料のSn、Inある
いはFeなどの元素を微量添加した合金とし、セ
ラミツクス焼成時に微量添加元素が合金表面に析
出して形成した選択酸化物によつて、セラミツク
スと貴金属材料とを化学結合させる方法がとられ
ている。 For example, the mainstream of dental prosthetic restorations is an aesthetically pleasing material called metal-baked porcelain, which is made by bonding precious metal alloys and ceramics. In this case, the bonding between the two is achieved by using an alloy to which trace amounts of elements such as Sn, In, or Fe are added, and when the ceramics are fired, the trace amounts of added elements precipitate on the alloy surface and form selective oxides. A method of chemically bonding materials is used.
しかし最近では経済性の点あるいはセラミツク
スの強度を補う必要性から、弾性係数の高いNi
−Cr系、Co−Cr系、Fe系等の卑金属合金が利用
されている。 However, recently, due to economical reasons or the need to supplement the strength of ceramics, Ni, which has a high elastic modulus, has been used.
- Base metal alloys such as Cr-based, Co-Cr-based, and Fe-based are used.
［発明が解決しようとする問題点］
卑金属合金をセラミツクスとの複合材料に用い
た場合には、貴金属合金材料と同様の接合方法を
行うと、合金表面に析出する酸化物と合金並びに
セラミツクスとの密着性が悪いために、合金とセ
ラミツクスとが剥離し易く、良好な接合体が得ら
れない。[Problems to be Solved by the Invention] When a base metal alloy is used in a composite material with ceramics, if the same bonding method as for the noble metal alloy material is performed, oxides precipitated on the alloy surface and the alloy and ceramics may be bonded together. Due to poor adhesion, the alloy and ceramics tend to separate, making it impossible to obtain a good bonded body.
［問題点を解決するための手段］
本発明は上記問題点を解決するためのものであ
り、卑金属合金成形体の表面に合金とセラミツク
スとの双方に接合し易い酸化物層を形成すること
によつて良好な接合体を得るものである。[Means for Solving the Problems] The present invention is intended to solve the above problems, and involves forming an oxide layer on the surface of a base metal alloy compact that is easily bonded to both the alloy and ceramics. As a result, a good bonded body can be obtained.
すなわち、本発明の第１発明は卑金属合金成形
体表面に金属クロムをスパツタリングにより積層
した後、加熱して卑金属合金と金属クロムとを反
応させて、表面に緻密な酸化層を形成し、ついで
セラミツクスと接合することを特徴とする金属と
セラミツクスとの接合方法である。又、第２発明
は第１発明において表面に緻密な酸化層を形成し
たのち酸化ケイ素をスパツタリングする方法であ
る。 That is, the first aspect of the present invention is to layer metallic chromium on the surface of a base metal alloy compact by sputtering, and then heat the base metal alloy to react with the metallic chromium to form a dense oxide layer on the surface. This is a method for joining metal and ceramics, which is characterized by joining with. The second invention is a method of forming a dense oxide layer on the surface of the first invention and then sputtering silicon oxide.
卑金属合金としてはNi−10〜20％Cr系、Co−
Cr系、Fe系などの合金が用いられる。Fe系合金
の一例としてはFe33〜40％、Ni17〜20％、Cr17
〜20％、Co17〜20％、Mn1.3〜1.5％、Si0.4〜0.5
％、Mo6〜10％の組成のものが挙げられる。そ
してスパツタリングにより形成する金属クロムの
膜厚は2000〜3000Åの範囲がよい。 Base metal alloys include Ni-10~20% Cr, Co-
Alloys such as Cr-based and Fe-based are used. Examples of Fe-based alloys include Fe33~40%, Ni17~20%, Cr17
~20%, Co17~20%, Mn1.3~1.5%, Si0.4~0.5
%, Mo6 to 10%. The thickness of the metallic chromium film formed by sputtering is preferably in the range of 2000 to 3000 Å.
この金属クロム膜は大気中で800℃で２時間程
度加熱してCr2O3酸化物層に変化させる。 This metallic chromium film is heated in the atmosphere at 800° C. for about 2 hours to transform it into a Cr 2 O 3 oxide layer.
又、第２発明においてはさらにその上にSiO2
のスパタリング被膜を形成する。 Moreover, in the second invention, SiO 2 is further added thereon.
A sputtering film is formed.
ついでセラミツクス素地を酸化物層に密着させ
て焼結する。使用するセラミツクスは例えば歯科
用の場合、SiO2、Al2O3、K2O、ZrO2などを主成
分とするフリツト磁器が挙げられる。その他耐熱
性セラミツクス材料等が挙げられる。 Then, the ceramic base is brought into close contact with the oxide layer and sintered. Examples of ceramics used include fritted porcelain whose main components are SiO 2 , Al 2 O 3 , K 2 O, ZrO 2 and the like in the case of dental use. Other examples include heat-resistant ceramic materials.
［作用］
卑金属合金成形体表面に積層した金属クロムを
加熱することにより、金属クロムが酸化物に変化
する過程で、合金から析出した酸化物と反応し、
Cr2O3を主成分とした緻密な酸化物層が合金表面
に形成される。この層がセラミツクス層を接合さ
せるための密着性を良くする。又、さらにSiO2
のスパツタリング層を複合させることによつても
良好な密着性が得られる。[Function] By heating the metallic chromium layered on the surface of the base metal alloy compact, in the process of changing the metallic chromium into an oxide, it reacts with the oxide precipitated from the alloy,
A dense oxide layer mainly composed of Cr 2 O 3 is formed on the alloy surface. This layer improves adhesion for bonding the ceramic layers. Furthermore, SiO 2
Good adhesion can also be obtained by combining sputtering layers.
［実施例］
実施例 １
Ni−20wt％Cr合金を用いロストワツクス法に
より歯科用材料を作製した。次にセラミツクスと
の接合面を細いエメリペーパーで均一に仕上げ、
アルコールにて脱脂および超音波洗浄後、900℃
で５分間加熱の前処理を施す。この前処理は鋳造
応力の緩和、鋳造時の偏析除去ならびにスパツタ
層と合金側酸化物との密着性を考慮した操作であ
るが、セラミツクとの密着性に関しては、かかる
前処理を施さなくても十分所期の効果を達成し得
る。[Examples] Example 1 A dental material was produced using a Ni-20wt%Cr alloy by the lost wax method. Next, finish the joint surface with the ceramics evenly with thin emery paper.
After degreasing with alcohol and ultrasonic cleaning, 900℃
Perform pretreatment by heating for 5 minutes. This pretreatment is an operation that takes into consideration the relaxation of casting stress, the removal of segregation during casting, and the adhesion between the spatter layer and the oxide on the alloy side. The desired effect can be fully achieved.
次に前処理後の合金材表面にスパツタリング装
置を用いて金属クロムを2000〜3000Åの膜厚にな
るようにスパツタリングする。スパツタ後800℃
の大気中雰囲気で２時間加熱する。その際金属ク
ロムが酸化物に変化する過程で、合金から析出し
た酸化物と反応し、Cr2O3を主成分とした緻密な
酸化物層が合金表面に形成される。 Next, metal chromium is sputtered onto the pretreated surface of the alloy material using a sputtering device to a film thickness of 2000 to 3000 Å. 800℃ after sputtering
Heat for 2 hours in an air atmosphere. During this process, metallic chromium reacts with oxides precipitated from the alloy, forming a dense oxide layer mainly composed of Cr 2 O 3 on the alloy surface.
上記の方法により形成した酸化物層に、SiO2、
Al2O3、K2O、ZrO2を主成分とする歯科用セラミ
ツクスを被覆して800℃にて焼成した。 SiO 2 ,
It was coated with dental ceramics containing Al 2 O 3 , K 2 O, and ZrO 2 as main components and fired at 800°C.
第１図ａはCr2O3酸化物層を形成したときの電
子顕微鏡（日立製Ｈ−700型）写真と線分析
（KEVEX社製の分析器7000Qによる）結果を示
すものである。この結果からCrがCr2O3に変化す
る過程でNiOと反応した酸化層を形成しているも
のと考えられる。 FIG. 1a shows an electron microscope photograph (model H-700 manufactured by Hitachi) and the results of line analysis (analyzer 7000Q manufactured by KEVEX) when a Cr 2 O 3 oxide layer was formed. From this result, it is considered that Cr reacts with NiO to form an oxide layer in the process of changing to Cr 2 O 3 .
第１図ｂはセラミツクスを焼成したものの電子
顕微鏡写真と線分析結果を示すもので、Cr2O3層
のピークは、セラミツクス焼成前（第１図ａ）に
比べてブロードになることから、Cr2O3とセラミ
ツクス側のSiO2、K2Oなどと拡散層を形成して
接着しているものと考えられる。 Figure 1b shows an electron micrograph and line analysis results of fired ceramics.The peak of the Cr 2 O 3 layer is broader than that before firing the ceramic (Fig. 1a), so it is clear that Cr It is thought that 2 O 3 and SiO 2 , K 2 O, etc. on the ceramic side form a diffusion layer and adhere to each other.
上記の方法により第２図ａ並びにｂに示すよう
な合金１とセラミツクス２との接合試験片をつく
り、引張試験を行つたところ、接合強さは117〜
140Kgｆ／cm2の値を示し、かつ破断状況も界面で
剥離せず、セラミツクス部で破断して良好な接合
体が得られた。 Bonding test pieces of Alloy 1 and Ceramics 2 as shown in Figures 2a and 2b were made by the above method and a tensile test was conducted, and the bonding strength was 117~
It showed a value of 140 Kgf/cm 2 , and a good bonded body was obtained with no peeling at the interface and rupture at the ceramic part.
実施例 ２
Fe：33.5wt％、Ni：19.5wt％、Cr：19.5wt％、
Co：19.5wt％、Mo：6.0wt％、Mn：1.5wt％、
Si：0.5wt％よりなるオーステナイト系合金を用
い、他は実施例１と同様にしてセラミツクスと接
合した。Example 2 Fe: 33.5wt%, Ni: 19.5wt%, Cr: 19.5wt%,
Co: 19.5wt%, Mo: 6.0wt%, Mn: 1.5wt%,
An austenitic alloy consisting of 0.5 wt% Si was used, and the other conditions were the same as in Example 1 to bond it to ceramics.
第３図ａは合金表面にCr2O3酸化物層を形成し
たときの電子顕微鏡写真並びに線分析結果を示す
もので、Cr2O3酸化物層には合金側から酸化した
Fe2O3も含まれており、反応酸化層が形成された
ものと考えられる。第３図ｂはセラミツクスと焼
成接合したものについてのものであり、線分析結
果ではCr2O3とFe2O3を主とした酸化層がセラミ
ツクスに含まれているSiO2、K2Oなどと拡散層
を形成している様子がうかがわれる。 Figure 3a shows an electron micrograph and line analysis results when a Cr 2 O 3 oxide layer was formed on the alloy surface.
Fe 2 O 3 was also included, and it is thought that a reactive oxidation layer was formed. Figure 3b shows the result of firing bonding with ceramics, and the line analysis results show that the ceramics contains an oxide layer mainly composed of Cr 2 O 3 and Fe 2 O 3 , such as SiO 2 , K 2 O, etc. It can be seen that a diffusion layer is formed.
この条件のものについて実施例１と同様に引張
試験を行つたところ、103〜177Kgｆ／cm2の値で、
破断強度も界面剥離せず、セラミツクス部で破断
した。 When a tensile test was conducted on this condition in the same manner as in Example 1, the value was 103 to 177 Kgf/ cm2 ,
Regarding the breaking strength, there was no interfacial peeling, and the ceramic part broke.
実施例 ３
実施例１においてCr2O3を主成分とした緻密な
酸化物層を形成した後、SiO2層をスパツタリン
グにより形成した。Example 3 After forming a dense oxide layer mainly composed of Cr 2 O 3 in Example 1, a SiO 2 layer was formed by sputtering.
その表面に実施例１と同様にセラミツクス層を
形成したところ、合金材とセラミツクスと良好な
接合体が得られた。 When a ceramic layer was formed on the surface in the same manner as in Example 1, a good bonded body of the alloy material and ceramics was obtained.
比較例 １
Ni−20wt％Cr合金を用いて実施例１と同様に
して歯科用材料をつくり、前処理を施した。次に
前処理後の合金材表面にスパツタリング装置を用
いてCr2O3層をスパツタリングにより形成した。Comparative Example 1 A dental material was prepared in the same manner as in Example 1 using a Ni-20wt%Cr alloy, and pretreated. Next, a Cr 2 O 3 layer was formed by sputtering on the pretreated alloy material surface using a sputtering device.
この上に実施例１と同様に歯科用セラミツクス
層を形成し、同様の試験をしたところ、界面で剥
離がおこつた。 When a dental ceramic layer was formed on this layer in the same manner as in Example 1 and the same test was conducted, peeling occurred at the interface.
［発明の効果］
本発明によれば卑金属合金成形体とセラミツク
スとの良好な接合体が容易に得られ、歯科用材料
あるいは耐熱高強度材料などの製造に有用であ
る。[Effects of the Invention] According to the present invention, a good joined body of a base metal alloy molded body and ceramics can be easily obtained, and it is useful for manufacturing dental materials or heat-resistant high-strength materials.
第１図ａは実施例１におけるCr2O3酸化物層を
形成したときの結晶の構造を示す電子顕微鏡写真
とオシロ波形、第１図ｂはセラミツクスを接合し
たときの結晶の構造を示す電子顕微鏡写真とオシ
ロ波形、第２図ａは試験片の平面図、同ｂは側面
図、第３図ａは実施例２の製品の結晶の構造を示
す電子顕微鏡写真とオシロ波形、第３図ｂは同じ
くセラミツクスを接合したときの結晶の構造を示
す電子顕微鏡写真とオシロ波形をそれぞれ示す。
１……合金、２……セラミツクス。
Figure 1a is an electron micrograph and oscilloscope waveform showing the crystal structure when forming the Cr 2 O 3 oxide layer in Example 1, and Figure 1b is an electron micrograph showing the crystal structure when ceramics are bonded. Microscope photograph and oscilloscope waveform, Figure 2a is a plan view of the test piece, Figure 3b is a side view, Figure 3a is an electron microscope photograph and oscilloscope waveform showing the crystal structure of the product of Example 2, Figure 3b Also shows an electron micrograph and an oscilloscope waveform showing the crystal structure when ceramics are bonded. 1...alloy, 2...ceramics.
Claims (1)
タリングにより積層した後、加熱して卑金属合金
と金属クロムとを反応させて、表面に緻密な酸化
層を形成し、ついでセラミツクスと接合すること
を特徴とする金属とセラミツクスの接合方法。 ２ 卑金属合金がNi−Cr系、Co−Cr系、Fe系の
合金である特許請求の範囲第１項記載の金属とセ
ラミツクスとの接合方法。 ３ スパツタリングにより形成する金属クロムの
膜厚が2000〜3000Åである特許請求の範囲第１項
記載の金属とセラミツクスとの接合方法。 ４ 卑金属合金成形体表面に金属クロムをスパツ
タリングにより積層した後、加熱して卑金属合金
と金属クロムとを反応させて、表面に緻密な酸化
層を形成し、さらに酸化ケイ素をスパツタリング
により積層し、ついでセラミツクスと接合するこ
とを特徴とする金属とセラミツクスとの接合方
法。 ５ 卑金属合金がNi−Cr系、Co−Cr系、Fe系の
合金である特許請求の範囲第４項記載の金属とセ
ラミツクスとの接合方法。 ６ スパツタリングにより形成する金属クロムの
膜厚が2000〜3000Åである特許請求の範囲第４項
記載の金属とセラミツクスとの接合方法。[Claims] 1. After laminating metallic chromium on the surface of a base metal alloy compact by sputtering, heating causes the base metal alloy and metallic chromium to react, forming a dense oxide layer on the surface, and then bonding with ceramics. A method for joining metal and ceramics, characterized by: 2. The method of joining metal and ceramics according to claim 1, wherein the base metal alloy is a Ni-Cr based, Co-Cr based, or Fe based alloy. 3. The method of joining metal and ceramics according to claim 1, wherein the metal chromium film formed by sputtering has a thickness of 2000 to 3000 Å. 4 After laminating metal chromium on the surface of the base metal alloy molded body by sputtering, heating the base metal alloy and metal chromium to react to form a dense oxide layer on the surface, and then layering silicon oxide by sputtering, and then A method for joining metal and ceramics, characterized by joining with ceramics. 5. The method of joining metal and ceramics according to claim 4, wherein the base metal alloy is a Ni-Cr based, Co-Cr based, or Fe based alloy. 6. The method of joining metal and ceramics according to claim 4, wherein the metal chromium film formed by sputtering has a thickness of 2000 to 3000 Å.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6129887A JPS63230576A (en) | 1987-03-18 | 1987-03-18 | Metal-ceramic joining method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6129887A JPS63230576A (en) | 1987-03-18 | 1987-03-18 | Metal-ceramic joining method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63230576A JPS63230576A (en) | 1988-09-27 |
| JPH0458431B2 true JPH0458431B2 (en) | 1992-09-17 |
Family
ID=13167145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6129887A Granted JPS63230576A (en) | 1987-03-18 | 1987-03-18 | Metal-ceramic joining method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63230576A (en) |
-
1987
- 1987-03-18 JP JP6129887A patent/JPS63230576A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63230576A (en) | 1988-09-27 |
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