CN103449846A - Formula for high-strength metallization of ceramic vacuum switch tube and application method thereof - Google Patents
Formula for high-strength metallization of ceramic vacuum switch tube and application method thereof Download PDFInfo
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Abstract
The invention aims to provide a high-packaging-strength formula for high-strength metallization of a ceramic vacuum switch tube and an application method thereof. The technical scheme is as follows: main and auxiliary components are mixed, and a paste adhesive is added to prepare a metallization paste; a high-strength metallized ceramic tube shell is manufactured by a special metallization technique. The main components comprise molybdenum powder, manganese powder, aluminum oxide, silicon dioxide powder and the like. The application method of the formula comprises the following steps: 1. proportioning; 2. mix grinding; 3. paste preparation; 4. pretreatment on ceramic application surface; 5. forming and sintering; 6. after-treatment of metallization; 7. electroplating; 8. testing. The invention can implement high-strength ceramic metallization; the test by an ASTM (American Society for Testing and Materials) method indicates that the average tensile strength is up to 250-450 MPa.
Description
Technical field
The present invention relates to the ceramic metallization technical field, be specifically related to a kind of compoistion and method of use for the ceramic vacuum switch pipe high-strength metal.
Background technology
For make pottery and metal carry out sealing-in or make ceramic surface have conductivity need be on ceramic surface the coating layer of metal, this technique is called ceramic metallization.The invention belongs to Al in the vacuum electronic technology
2o
3the Ceramic-to-Metal sealing-in.The pottery that the aluminum oxide of take is main component, be called alumina ceramics, as A-93 porcelain, A-95 porcelain, A-97 porcelain, A-99 porcelain etc.Its principal crystalline phase is α-Al
2o
3.The characteristics such as alumina ceramics has that physical strength is high, dielectric properties are excellent under high temperature, vacuum-tightness is good, dielectric loss is low, hardness is large, thermal conductivity is good, high temperature resistant, wear-resisting, corrosion-resistant, anti-oxidant, be mainly used in making ultra-high frequency, large power, electrically vacuum device insulation system part, thick film, film and microwave and Microwave integrated circuit substrate, the housing of silicon rectifier and support, radome etc.
The composition of vacuum switch tube ceramic metallization coating is all molybdenum manganese paste.The main quality index of ceramic metallization is the tensile strength of peeling off of Ceramic-to-Metal layer.At home, by vacuum electronic industry standard SJ/T11246-2001 " the effective ceramic cartridge of vacuum switch " requirement, answer >=the 90MPa(of average tensile strength value of standard tensile members method test will revise as 100MPa), the answer >=120MPa(of average tensile strength value of three point method (ASTM method) test will revise as 130MPa).In the world, the standard of Siemens is the answer >=250MPa of average tensile strength value of ASTM method test, and the standard of Korea S KCC company is the answer >=420MPa of average tensile strength value of ASTM method test.The ceramic metallization state of the art of visible China need to improve.Huadong Photoelectric Technique Institute of Anhui Province's disclosure of the invention number: 101538170, " a kind of compoistion and method of use for ceramic metallization ", sealing-in metallization aperture sealing strength reaches 300----400MPa, but aperture, hole depth are not quite clear, and test condition is much better than the ASTM method.
Summary of the invention
The object of the present invention is to provide the formula for the ceramic vacuum switch pipe high-strength metal and using method thereof that a kind of package strength is high.
Technical problem to be solved by this invention be to provide a kind of package strength high (ASTM method test average tensile strength value 250----450MPa) for A-93~metallized compoistion and method of use of A-97 alumina-ceramic.
The objective of the invention is to be achieved through the following technical solutions: mixed by main component and auxiliary material, then add paste glue, make metallizing paste; Adopt distinctive metallization process to manufacture the high-strength metal ceramic cartridge.
In described metallizing paste, predominant quantity is than as follows: 70~78 parts of molybdenum powders, 9~13 parts of manganese powders, 6~8 parts of aluminium sesquioxides, 7~9 parts of silicon dioxide powders;
In described metallizing paste, auxiliary material weight is one or more the combination in following component, each component and auxiliary material with predominant quantity than as follows: calcium oxide weight 0~2%, magnesium oxide weight 0~1.5% and titanium dioxide weight 0~1%.
The purity of molybdenum powder, manganese powder is greater than 99.9%, the purity of aluminium oxide powder, silicon dioxide powder is greater than 99.5%, the mean diameter of molybdenum powder is 1.5-2.5 μ m, and the mean diameter of manganese powder is 2~3 μ m, and the maximum diameter of aluminium sesquioxide≤5 μ m and submicron order are 1~3%.
The concrete steps of the using method of above-mentioned formula are as follows:
(1) batching: take molybdenum powder, manganese powder, aluminium oxide powder, silicon dioxide powder, then add auxiliary material;
(2) mix grinding: the pulvis of step (1) is mixed with ethanol, and ethanol weight is 1~1.5 times of pulvis weight, and mixed solution is carried out to mix grinding, mix grinding 1200~1800min in 30~40r/min general milling machine; Put into again afterwards 300~400r/min planetary ball mill, 600~900min;
After mix grinding finishes, suspension is placed in to ultrasonic wave and is vibrated 25~35min, then dry in baking oven, temperature is more than 80 ℃, and drying time keeps approximately every 40~60min, stirring once in 240~300min and drying course, seals the material powder after oven dry up for safekeeping;
(3) paste preparation:
Preparation paste glue: 1 part of binding agent is joined in 18~20 parts of solvents, heating while stirring, Heating temperature is 80~100 ℃, adjusts viscosity as follows: manual painting cream is 0.07~0.1pa.s by the viscosity of glue, and silk screen printing is 2~6pa.s by the viscosity of glue;
Add paste glue in the metallization powder made in step (2), paste is 25~30% of metallization powder gross weight by the weight that adds of glue, in vibromill or planetary ball mill, is mixed 240~480min;
(4) the ceramic coated face is carried out to pre-treatment
Use varigrained emery wheel or abrasive material, control the roughness of ceramic coated face in Ra0.5~Ra1.6, porosity 20%~40%;
(5) moulding sintering
Porcelain piece is coated with cream and applies one to twice, porcelain piece should be dried after being coated with cream, after will being coated with cream afterwards and the porcelain piece of having dried carry out sintering;
(6) metallization aftertreatment
Pottery after sintering is at room temperature soaked 10~20 seconds in 40~50%HCl concentration solution;
(7) electroplate
The product of step 6 is electroplated take in the electroplate liquid that single nickel salt is main salt;
(8) test
Tensile strength with ASTM method test metallized ceramic.
Wherein, the whole components described in step (1) need fully dry, and drying mode is at baking oven inner drying more than 80 ℃ and keeps 240~300mim.
In step (2), the abrading-ball in general milling machine and planetary ball mill is zirconia ball, high aluminium ball or agate ball.
The concrete steps of step (5) moulding are: the difference, paste kind, the coating method that apply position according to porcelain piece are selected the manual cream that is coated with of suitable painting pen.Silk screen printing, for adopting 80~160 purpose stainless (steel) wires, applies one to twice.
In step (5), the condition of sintering is: 1430~1470 ℃ of temperature advance continuously course 360~480min in pushed bat kiln; The sintering atmosphere is the hydrogen-nitrogen mixture gas that ammonia decomposes, 30~40 ℃ of dew points.
The concrete mode that step (7) is electroplated is: electroplating work procedure carries out as quickly as possible after metallization completes.Plating is carried out in as main salt electroplate liquid usining single nickel salt.Electroplating time is 20~30min, and thickness of coating is 1~6 μ m.
Advantage of the present invention is as follows:
1, the molybdenum manganese metal paste that the present invention uses is (to be Mo, Mn, Al to common metallizing formula component
2o
3, SiO
2) adopt empirical algorithms to determine the weight percent of each component.
2, after detecting the matrix ceramic composition, with contained MgO, CaO, TiO in pottery
2weight percent etc. component is radix, adopts the multifactorial experiment positive arrearing optimization to find out interpolation assistant agent MgO, CaO, the TiO of molybdenum manganese metal paste
2the coupling number of weight percent, to obtain high-strength ceramic metallization (the average tensile strength value of ASTM method test reaches 250~450MPa).
3, make binding agent with carboxyethyl cellulose, with Terpineol 350, make solvent, control suitable viscosity number, can be simultaneously for manual painting cream and silk screen printing.
4, the ceramic coated face is carried out to pre-treatment, rationally control roughness and porosity to strengthen the Ceramic-to-Metal bonding strength.
Metallization technology of the present invention because sintering temperature is low, large, the sealing strength of density and reliability high, thereby the method for metallising of alternative common use, reach 250~450MPa(ASTM method to A-93~A-97 alumina ceramics metallization tensile strength).
Embodiment
Embodiment 1
Pottery: A-93
In described metallizing paste, predominant quantity is than as follows: 75 parts of molybdenum powders, 11 parts of manganese powders, 6 parts of aluminium oxide powders, 8 parts of silicon dioxide powders.
The interpolation weight of the composition of auxiliary material and the weight ratio of predominant quantity are as follows: calcium oxide weight 2%, magnesium oxide weight 0.5% and titanium dioxide weight 0.5%.
Wherein, the purity of molybdenum powder, manganese powder is greater than 99.9%, and the purity of aluminium oxide powder, silicon dioxide powder is greater than 99.5%; The mean diameter of molybdenum powder is 2.2 μ m, and the mean diameter of manganese powder is 2.5 μ m, and the maximum diameter of aluminium sesquioxide≤5 μ m and submicron order are 2%.
Binding agent is carboxyethyl cellulose, and solvent is Terpineol 350.
Adopt said components to be produced in conjunction with following using method:
(1) batching: take molybdenum powder, manganese powder, aluminium oxide powder, silicon dioxide powder, then add auxiliary material; Fully dry afterwards, drying mode is at 85 ℃ of baking oven inner dryings and keeps 240mim.
(2) mix grinding: the pulvis in step 1 mixes with ethanol, and ethanol weight is 1.5 times of pulvis weight, and mixed solution is carried out to mix grinding, mix grinding 1200min in 40r/min general milling machine; Put into again afterwards 300r/min planetary ball mill 900min; Abrading-ball in general milling machine and planetary ball mill is zirconia ball.
After mix grinding finishes, suspension is placed in to ultrasonic wave and is vibrated 35min, then dry in baking oven, temperature is more than 85 ℃, and drying time keeps every one hour, stirring once in about 300min and drying course, seals the material powder after oven dry up for safekeeping;
(3) paste preparation:
Preparation paste glue: 1 part of carboxyethyl cellulose is joined in 20 parts of Terpineol 350s, heating while stirring, Heating temperature is 90 ℃, the viscosity of regulating glue is 3pa.s;
The metallization powder that step (2) is made, add paste glue, and paste is 30% of metallization sub-material gross weight by the weight added of glue, in vibromill or planetary ball mill, is mixed 240min;
(4) the ceramic coated face is carried out to pre-treatment
Use varigrained emery wheel or abrasive material, control the roughness of ceramic coated face in Ra0.8, porosity 20%~40%;
(5) moulding sintering
Be coated with the cream mode for being silk screen printing: silk screen printing employing stainless (steel) wire, mesh adopts 160 orders, applies twice.Porcelain piece is being coated with the cream post-drying.After will being coated with cream afterwards and the porcelain piece of having dried carry out sintering; The condition of sintering is: 1450 ℃ of temperature advance continuously course 360min in pushed bat kiln; The sintering atmosphere is hydrogen-nitrogen mixture gas, and hydrogen, nitrogen volume ratio are 3: 1,30 ℃ of dew points.
(6) metallization aftertreatment
Pottery after sintering is at room temperature soaked 10 seconds in 50%HCl concentration solution;
(7) electroplate
The product of step 6 is electroplated take in the electroplate liquid that single nickel salt is main salt; Electroplating time is 20min, and thickness of coating is 3 μ m.
(8) test
Tensile strength with ASTM method test metallized ceramic.
(8) test (diameter 3mm can cut down bar)
Numbering | F(N) | σ(MPa) |
1 | 2592 | 367 |
2 | 3191 | 452 |
3 | 3018 | 427 |
Embodiment 2
Pottery: A-95
In described metallizing paste, predominant quantity is than as follows: 73 parts of molybdenum powders, 11 parts of manganese powders, 7 parts of aluminium sesquioxides, 9 parts of silicon dioxide powders;
The interpolation weight of the composition of auxiliary material and the weight ratio of predominant quantity are as follows: calcium oxide weight 2%, magnesium oxide weight 1%.
Wherein, the purity of molybdenum powder, manganese powder is greater than 99.9%, and the purity of aluminium oxide powder, silicon dioxide powder is greater than 99.5%; The mean diameter of molybdenum powder is 1.5~2.5 μ m, and the mean diameter of manganese powder is 2~3 μ m, and the maximum diameter of aluminium sesquioxide≤5 μ m and submicron order are 1~3%.
Binding agent is carboxyethyl cellulose, and solvent is Terpineol 350.
Adopt said components to be produced in conjunction with following using method:
(1) batching: take molybdenum powder, manganese powder, aluminium oxide powder, silicon dioxide powder, then add auxiliary material; Fully dry afterwards, drying mode is at 90 ℃ of baking oven inner dryings and keeps 300mim.
(2) mix grinding: the pulvis in step 1 mixes with ethanol, and ethanol weight is 1.2 times of pulvis weight, and mixed solution is carried out to mix grinding, mix grinding 1500min in 30r/min general milling machine; Put into again afterwards 400r/min planetary ball mill 720min; Abrading-ball in general milling machine and planetary ball mill is high aluminium ball.
After mix grinding finishes, suspension is placed in to ultrasonic wave and is vibrated 35min, then dry in baking oven, temperature is 90 ℃, and drying time keeps every one hour, stirring once in about 240min and drying course, seals the material powder after oven dry up for safekeeping;
(3) paste preparation:
Preparation paste glue: 1 part of carboxyethyl cellulose is joined in 20 parts of Terpineol 350s, heating while stirring, Heating temperature is 100 ℃, adjusting viscosity is 2.5pa.s;
The metallization powder that step (2) is made, add paste glue, and paste is 30% of metallization powder gross weight by the weight added of glue, in vibromill or planetary ball mill, is mixed 300min;
(4) the ceramic coated face is carried out to pre-treatment
Use varigrained emery wheel or abrasive material, control the roughness of ceramic coated face in Ra0.8, porosity 20%~40%;
(5) moulding sintering
Being coated with the cream mode is silk screen printing: adopt stainless (steel) wire, mesh adopts 120 orders, applies twice.Porcelain piece is being coated with the cream post-drying, after will being coated with cream afterwards and the porcelain piece of having dried carry out sintering; The condition of sintering is: 1470 ℃ of temperature advance continuously course 360min in pushed bat kiln; The sintering atmosphere is hydrogen-nitrogen mixture gas, and hydrogen, nitrogen volume ratio are 3: 1,35 ℃ of dew points.
(6) metallization aftertreatment
Pottery after sintering is at room temperature soaked 15 seconds in 50%HCl concentration solution;
(7) electroplate
The product of step 6 is electroplated take in the electroplate liquid that single nickel salt is main salt; Electroplating time is 25min, and thickness of coating is 4 μ m.
(8) test
Tensile strength with ASTM method test metallized ceramic.
(8) test (diameter 3mm can cut down bar)
Numbering | F(N) | σ(MPa) |
1 | 2893 | 409 |
2 | 3320 | 469 |
3 | 3013 | 426 |
Embodiment 3
Pottery: A-96
In described metallizing paste, predominant quantity is than as follows: 78 parts of molybdenum powders, 9 parts of manganese powders, 6 parts of aluminium sesquioxides, 7 parts of silicon dioxide powders;
The interpolation weight of the composition of auxiliary material and the weight ratio of predominant quantity are as follows: magnesium oxide, main component weight 1.5%.
Wherein, the purity of molybdenum powder, manganese powder is greater than 99.9%, and the purity of aluminium oxide powder, silicon dioxide powder is greater than 99.5%; The mean diameter of molybdenum powder is 2.5 μ m, and the mean diameter of manganese powder is 3 μ m, and the maximum diameter of alchlor≤5 μ m and submicron order are 3%.
Binding agent is carboxyethyl cellulose, and solvent is Terpineol 350.
Adopt said components to be produced in conjunction with following using method:
(1) batching: take molybdenum powder, manganese powder, aluminium sesquioxide, silicon dioxide powder, then add auxiliary material; Fully dry afterwards, drying mode is at baking oven inner drying more than 80 ℃ and keeps 240mim.
(2) mix grinding: the pulvis in step (1) mixes with ethanol, and ethanol weight is 1.5 times of pulvis weight, and mixed solution is carried out to mix grinding, mix grinding 1500min in 35r/min general milling machine; Put into again afterwards 350r/min planetary ball mill 720min; Abrading-ball in general milling machine and planetary ball mill is agate ball.
After mix grinding finishes, suspension is placed in to ultrasonic wave and is vibrated 35min, then dry in baking oven, temperature is 90 ℃, and drying time keeps every one hour, stirring once in about 240min and drying course, seals the material powder after oven dry up for safekeeping;
(3) paste preparation:
Preparation paste glue: 1 part of carboxyethyl cellulose is joined in 20 parts of Terpineol 350s, heating while stirring, Heating temperature is 90 ℃, adjusting viscosity is 0.1pa.s;
The metallization powder that step (2) is made, add paste glue, and paste is 30% of metallization sub-material gross weight by the weight added of glue, in vibromill or planetary ball mill, is mixed 480min;
(4) the ceramic coated face is carried out to pre-treatment
Use varigrained emery wheel or abrasive material, control the roughness of ceramic coated face in Ra1.0, porosity 15%~30%;
(5) moulding sintering
Be coated with the cream mode for the manual cream that is coated with: select the high-quality writing brush, apply twice.Porcelain piece is being coated with the cream post-drying, after will being coated with cream afterwards and the porcelain piece of having dried carry out sintering; The condition of sintering is: 1470 ℃ of temperature advance continuously course 360min in pushed bat kiln; The sintering atmosphere is hydrogen-nitrogen mixture gas, and hydrogen, nitrogen volume ratio are 3: 1,40 ℃ of dew points.
(6) metallization aftertreatment
Pottery after sintering is at room temperature soaked 15 seconds in 50%HCl concentration solution;
(7) electroplate
The product of step 6 is electroplated take in the electroplate liquid that single nickel salt is main salt; Electroplating time is 20min, and thickness of coating is 3 μ m.
(8) test
Tensile strength with ASTM method test metallized ceramic.
(8) test (diameter 3mm can cut down bar)
Numbering | F(N) | σ(MPa) |
1 | 2720 | 385 |
2 | 2028 | 287 |
3 | 2190 | 310 |
Claims (8)
1. the formula for the ceramic vacuum switch pipe high-strength metal, is characterized in that: the metallizing paste that it is mixed and added paste to form with glue by main component and auxiliary material;
In described metallizing paste, predominant quantity is than as follows: 70~78 parts of molybdenum powders, 9~13 parts of manganese powders, 6~8 parts of aluminium sesquioxides, 7~9 parts of silicon dioxide powders;
In described metallizing paste, auxiliary material weight is one or more the combination in following component, each component and auxiliary material with predominant quantity than as follows: calcium oxide weight 0~2%, magnesium oxide weight 0~1.5% and titanium dioxide weight 0~1%.
2. the formula for the ceramic vacuum switch pipe high-strength metal according to claim 1, it is characterized in that: the purity of molybdenum powder, manganese powder is greater than 99.9%, and the purity of aluminium oxide powder, silicon dioxide powder is greater than 99.5%.
3. the formula for the ceramic vacuum switch pipe high-strength metal according to claim 1, it is characterized in that: the mean diameter of molybdenum powder is 1.5-2.5 μ m, the mean diameter of manganese powder is 2~3 μ m, and the maximum diameter of aluminium sesquioxide≤5 μ m and submicron order are 1~3%.
4. according to the described formula for the ceramic vacuum switch pipe high-strength metal of claim 1-3 and using method thereof, it is characterized in that:
(1) batching: take molybdenum powder, manganese powder, aluminium oxide powder, silicon dioxide powder, then add auxiliary material;
(2) mix grinding: the pulvis of step (1) is mixed with ethanol, and ethanol weight is 1~1.5 times of pulvis weight, and mixed solution is carried out to mix grinding, mix grinding 1200~1800min in 30~40r/min general milling machine; Put into again afterwards 300~400r/min planetary ball mill, 600~900min;
After mix grinding finishes, suspension is placed in to ultrasonic wave and is vibrated 25~35min, then dry in baking oven, temperature is more than 80 ℃, and drying time keeps approximately every 40~60min, stirring once in 240~300min and drying course, seals the material powder after oven dry up for safekeeping;
(3) paste preparation:
Preparation paste glue: 1 part of binding agent is joined in 18~20 parts of solvents, heating while stirring, Heating temperature is 80~100 ℃, adjusts viscosity as follows: manual painting cream is 0.07~0.1pa.s by the viscosity of glue, and silk screen printing is 2~6pa.s by the viscosity of glue;
Add paste glue in the metallization powder made in step (2), paste is 25~30% of metallization powder gross weight by the weight that adds of glue, in vibromill or planetary ball mill, is mixed 240~480min;
(4) the ceramic coated face is carried out to pre-treatment
Use varigrained emery wheel or abrasive material, control the roughness of ceramic coated face in Ra0.5~Ra1.6, porosity 20%~40%;
(5) moulding sintering
Porcelain piece is coated with cream and applies one to twice, porcelain piece should be dried after being coated with cream, after will being coated with cream afterwards and the porcelain piece of having dried carry out sintering;
(6) metallization aftertreatment
Pottery after sintering is at room temperature soaked 10~20 seconds in 40~50%HCl concentration solution;
(7) electroplate
The product of step 6 is electroplated take in the electroplate liquid that single nickel salt is main salt;
(8) test
Tensile strength with ASTM method test metallized ceramic.
5. the formula for the ceramic vacuum switch pipe high-strength metal according to claim 4 and using method thereof, it is characterized in that: the whole component needs described in step (1) are fully dry, and drying mode is at baking oven inner drying more than 80 ℃ and keeps 240~300mim.
6. the formula for the ceramic vacuum switch pipe high-strength metal according to claim 4 and using method thereof, it is characterized in that: in step (5), the condition of sintering is: 1430~1470 ℃ of temperature advance continuously course 360~480min in pushed bat kiln; The sintering atmosphere is the hydrogen-nitrogen mixture gas that ammonia decomposes, 30~40 ℃ of dew points.
7. the formula for the ceramic vacuum switch pipe high-strength metal according to claim 4, it is characterized in that: described binding agent is carboxyethyl cellulose.
8. the formula for the ceramic vacuum switch pipe high-strength metal according to claim 4, it is characterized in that: described solvent is Terpineol 350.
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