CN111063499B - Preparation method of annular piezoresistor vacuum sputtering copper electrode made of zinc oxide material - Google Patents
Preparation method of annular piezoresistor vacuum sputtering copper electrode made of zinc oxide material Download PDFInfo
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- CN111063499B CN111063499B CN201911423292.9A CN201911423292A CN111063499B CN 111063499 B CN111063499 B CN 111063499B CN 201911423292 A CN201911423292 A CN 201911423292A CN 111063499 B CN111063499 B CN 111063499B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
- H01C7/105—Varistor cores
- H01C7/108—Metal oxide
- H01C7/112—ZnO type
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/28—Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals
Abstract
The invention relates to a preparation method of an annular piezoresistor electrode; in particular to a preparation method of an annular piezoresistor vacuum sputtering copper electrode made of zinc oxide material, which comprises the following steps: step one, preparing bismuth oxide into slurry with the mass concentration of 10-15%; step two, printing the slurry prepared in the step one to the top surface and the bottom surface of the annular zinc oxide ceramic body in a screen printing mode; thirdly, sintering the product obtained in the second step at high temperature to form a pressure-sensitive junction on the surfaces of the bismuth oxide and zinc oxide ceramic bodies; and step four, placing the product prepared in the step three into vacuum sputtering coating equipment, shielding the position of a polar opening of the annular piezoresistor, firstly sputtering a nickel-chromium alloy transition layer of 1.8 microns by using nickel-chromium alloy, and then sputtering a copper electrode of 2.8 microns by using metal copper. The invention improves the performance of the annular piezoresistor and saves the production cost at the same time.
Description
Technical Field
The invention relates to a preparation method of an annular piezoresistor electrode; in particular to a preparation method of an annular piezoresistor vacuum sputtering copper electrode made of zinc oxide.
Background
At present, the annular piezoresistor made of zinc oxide generally adopts a silver electrode, and the preparation process comprises the following steps: the bismuth oxide is directly added into the silver paste, is printed on the surface of the zinc oxide ceramic body through screen printing, and is fused and permeated into the zinc oxide ceramic body after high-temperature sintering for a certain time, and meanwhile, a junction boundary with pressure-sensitive characteristics, namely a pressure-sensitive junction for short, is generated. Although the preparation process is simple, silver is a noble metal, the cost is high, and the ohmic contact characteristics of silver and zinc oxide are not optimal.
Disclosure of Invention
To solve the above technical problems, the present invention aims to: the preparation method of the zinc oxide annular piezoresistor vacuum sputtering copper electrode is provided, the performance of the annular piezoresistor is improved, and the production cost is saved.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the preparation method of the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material comprises the following steps:
step one, preparing bismuth oxide into slurry with the mass concentration of 10% -15%;
step two, printing the slurry prepared in the step one to the top surface and the bottom surface of the annular zinc oxide ceramic body in a screen printing mode;
thirdly, sintering the product obtained in the second step at high temperature to form a pressure-sensitive junction on the surfaces of the bismuth oxide and zinc oxide ceramic bodies;
and step four, placing the product prepared in the step three into vacuum sputtering coating equipment, shielding the position of a polar opening of the annular piezoresistor, firstly sputtering a nickel-chromium alloy transition layer of 1.8-2.3 microns by using nickel-chromium alloy, and then sputtering a copper electrode of 2.8-3.3 microns by using metal copper.
The invention uses copper electrode to replace silver electrode, the market price of copper is 40 yuan/kg, the market price of silver is 4 yuan/g, the product with the same specification greatly reduces the material cost. Considering that copper belongs to active metal and cannot be directly exposed in the atmosphere for high-temperature sintering and infiltrating, firstly, bismuth oxide slurry is screen-printed on the surface of zinc oxide, then, the high-temperature sintering and infiltrating are carried out, so that bismuth oxide is melted and combined with the zinc oxide to generate a pressure-sensitive junction, a vacuum sputtering mode is adopted to plate a copper electrode on the surface of a zinc oxide ceramic body after the pressure-sensitive junction is generated, oxygen does not participate in the whole process, the oxidation problem of copper is not worried about, and in order to enhance the combination strength between the zinc oxide ceramic body and the copper electrode, a nickel-chromium alloy transition layer of 1.8-2.3 micrometers is vacuum sputtered before the copper electrode is vacuum.
Preferably, in the second step, 300-mesh screen printing bismuth oxide slurry is adopted, and the thickness of the printing is 5-8 microns.
Preferably, in step four, the thickness of the nickel-chromium alloy transition layer is 2 microns.
Preferably, in step four, the copper electrode thickness is 3 microns.
Preferably, the specific process of the third step is as follows: and (3) sintering the product prepared in the step (II) by adopting a mesh belt resistance furnace, wherein the sintering temperature is as follows in sequence: heating at 300 ℃ for 10 minutes, heating at 500 ℃ for 10 minutes, heating at 700 ℃ for 10 minutes and heating at 850 ℃ for 10 minutes, wherein the melting point of bismuth oxide is 825 ℃, the bismuth oxide starts to infiltrate at about 720 ℃, and the bismuth oxide reaches a molten state after being heated in a high-temperature section of a mesh belt resistance furnace, so that a pressure-sensitive junction can be successfully generated.
Preferably, step two is performed by placing the ring piezoresistor on a printing table of a screen printing machine by means of a printing pallet.
Preferably, the printing support plate is provided with a plurality of circular accommodating grooves corresponding to the annular piezoresistors, the centers of the accommodating grooves are provided with limiting bulges corresponding to the center holes of the annular piezoresistors, the circular grooves are provided with 2-4 through holes on the bottom surfaces of the peripheries of the limiting bulges, the annular piezoresistors are fixed through a vacuum adsorption device during printing, the printing precision is prevented from being influenced by the annular pressure-sensitive displacement, the vacuum adsorption device can be a sucker connected with a vacuum pump, the sucker is adsorbed on the back surface of the printing support plate, and the annular piezoresistors are adsorbed and positioned through the through holes.
Preferably, when the step four is executed, the annular piezoresistor is placed in the vacuum sputtering coating equipment through the coating supporting plate, the upper surface of the coating supporting plate is covered with a shielding piece, and the shielding piece is used for shielding the position of the electrode opening of the annular piezoresistor, so that the sputtered slurry is prevented from polluting the electrode opening.
Preferably, the coating film layer board corresponds annular piezo-resistor and sets up a plurality of circular holding recesses, and the holding recess center corresponds annular piezo-resistor centre bore and sets up spacing arch, when placing annular piezo-resistor to the coating film layer board, can directly place a heap of annular piezo-resistor on the coating film layer board upper surface, then the horizontally coating film layer board that rocks, makes annular piezo-resistor fill up all holding recesses, annular piezo-resistor upper surface and coating film layer board upper surface parallel and level that the holding recess was put, remaining annular piezo-resistor directly pushes away from coating film layer board upper surface with the hand, easy operation is swift.
Compared with the prior art, the invention has the following beneficial effects:
the invention improves the performance of the annular piezoresistor and saves the production cost at the same time. The copper electrode is used for replacing the traditional silver electrode, the market price of copper is 40 yuan/kg, the market price of silver is 4 yuan/g, products with the same specification are obtained, the production cost is saved by 20%, the copper electrode and the zinc oxide ceramic body have better ohmic contact characteristics, the product performance is improved, and the ex-factory qualification rate of the annular piezoresistor prepared by the method is higher than 90% according to the verification.
Drawings
FIG. 1 is a schematic diagram of a printing pallet structure.
FIG. 2 is a schematic view of a structure of a coated supporting plate.
Fig. 3 is a schematic view of a structure of the shielding sheet.
Fig. 4 is a schematic diagram of the shielding effect of the shielding sheet.
In the figure: 1. printing a supporting plate; 2. an accommodating groove; 3. a limiting bulge; 4. a through hole; 5. coating a film supporting plate; 6. a shielding sheet.
Detailed Description
Example 1:
the preparation method of the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material comprises the following steps:
step one, preparing bismuth oxide into slurry with the mass concentration of 10%;
step two, printing the slurry prepared in the step one to the top surface and the bottom surface of the annular zinc oxide ceramic body in a screen printing mode;
thirdly, sintering the product obtained in the second step at high temperature to form a pressure-sensitive junction on the surfaces of the bismuth oxide and zinc oxide ceramic bodies;
and step four, placing the product prepared in the step three into vacuum sputtering coating equipment, shielding the position of a polar opening of the annular piezoresistor, firstly sputtering a nickel-chromium alloy transition layer of 1.8 microns by using nickel-chromium alloy, and then sputtering a copper electrode of 2.8 microns by using metal copper.
In the second step, 300-mesh screen printing bismuth oxide slurry is adopted, and the printing thickness is 5-8 microns; the specific process of the third step is as follows: and (3) sintering the product prepared in the step (II) by adopting a mesh belt resistance furnace, wherein the sintering temperature is as follows in sequence: heating at 300 ℃ for 10 minutes, heating at 500 ℃ for 10 minutes, heating at 700 ℃ for 10 minutes and heating at 850 ℃ for 10 minutes, wherein the melting point of bismuth oxide is 825 ℃, the bismuth oxide starts to infiltrate at about 720 ℃, and the bismuth oxide reaches a molten state after being heated in a high-temperature section of a mesh belt resistance furnace, so that a pressure-sensitive junction can be successfully generated.
When the second step is executed, the annular piezoresistor is placed on the printing table top of the screen printing machine through the printing support plate 1, as shown in fig. 1, a plurality of circular accommodating grooves 2 are formed in the printing support plate 1 corresponding to the annular piezoresistor, limiting bulges 3 are formed in the centers of the accommodating grooves 2 corresponding to the center holes of the annular piezoresistor, 2-4 through holes 4 are formed in the bottom surfaces of the peripheries of the limiting bulges 2, the annular piezoresistor is fixed through a vacuum adsorption device during printing, the printing precision is prevented from being influenced by the annular pressure-sensitive displacement, the vacuum adsorption device can be a sucker with a vacuum pump, the sucker is adsorbed on the back of the printing support plate 1, and the annular piezoresistor is adsorbed and positioned through the through holes 4.
When the fourth step is executed, the annular piezoresistor is placed in the vacuum sputtering coating equipment through the coating supporting plate 5, the upper surface of the coating supporting plate 5 is covered by the shielding sheet 6, the shielding sheet 6 is used for shielding the position of the pole opening of the annular piezoresistor and preventing sputtered slurry from polluting the pole opening, as shown in fig. 2-4, for example, a three-electrode annular piezoresistor is taken, the coating supporting plate 5 is provided with a plurality of circular accommodating grooves 2 corresponding to the annular piezoresistor, the centers of the accommodating grooves 2 are provided with limiting bulges 3 corresponding to the central holes of the annular piezoresistor, when the annular piezoresistor is placed on the coating supporting plate 5, a stack of annular piezoresistors can be directly placed on the upper surface of the coating supporting plate 5, then the coating supporting plate 5 is horizontally shaken to enable the annular piezoresistors to fill all the accommodating grooves 2, and the upper surface of the annular piezoresistor placed in the accommodating groove 2, the rest of the annular piezoresistors are directly pushed away from the upper surface of the coating supporting plate 5 by hands, and the operation is simple and rapid.
The invention uses copper electrode to replace silver electrode, the market price of copper is 40 yuan/kg, the market price of silver is 4 yuan/g, the product with the same specification greatly reduces the material cost. Considering that copper belongs to an active metal and cannot be directly exposed in the atmosphere for high-temperature sintering and infiltrating, firstly, bismuth oxide slurry is screen-printed on the surface of zinc oxide, then, the high-temperature sintering and infiltrating are carried out, so that bismuth oxide is melted and combined with the zinc oxide to generate a pressure-sensitive junction, a vacuum sputtering mode is adopted to plate a copper electrode on the surface of a zinc oxide ceramic body after the pressure-sensitive junction is generated, oxygen does not participate in the whole process, the oxidation problem of copper is not worried about, and in order to enhance the combination strength between the zinc oxide ceramic body and the copper electrode, a nickel-chromium alloy transition layer of 1.8 microns is vacuum sputtered before the copper electrode is.
Example 2:
the preparation method of the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material comprises the following steps:
step one, preparing bismuth oxide into slurry with the mass concentration of 12%;
step two, printing the slurry prepared in the step one to the top surface and the bottom surface of the annular zinc oxide ceramic body in a screen printing mode;
thirdly, sintering the product obtained in the second step at high temperature to form a pressure-sensitive junction on the surfaces of the bismuth oxide and zinc oxide ceramic bodies;
and step four, placing the product prepared in the step three into vacuum sputtering coating equipment, shielding the position of a polar opening of the annular piezoresistor, firstly sputtering a nickel-chromium alloy transition layer of 2 microns by using nickel-chromium alloy, and then sputtering a copper electrode of 3 microns by using metal copper.
Other process details of this example are the same as example 1.
Example 3:
the preparation method of the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material comprises the following steps:
step one, preparing bismuth oxide into slurry with the mass concentration of 15%;
step two, printing the slurry prepared in the step one to the top surface and the bottom surface of the annular zinc oxide ceramic body in a screen printing mode;
thirdly, sintering the product obtained in the second step at high temperature to form a pressure-sensitive junction on the surfaces of the bismuth oxide and zinc oxide ceramic bodies;
and step four, placing the product prepared in the step three into vacuum sputtering coating equipment, shielding the position of a polar opening of the annular piezoresistor, firstly sputtering a nickel-chromium alloy transition layer of 2.3 microns by using nickel-chromium alloy, and then sputtering a copper electrode of 3.3 microns by using metal copper.
Other process details of this example are the same as example 1.
Claims (7)
1. A preparation method of a zinc oxide annular piezoresistor vacuum sputtering copper electrode is characterized by comprising the following steps:
step one, preparing bismuth oxide into slurry with the mass concentration of 10% -15%;
step two, printing the slurry prepared in the step one to the top surface and the bottom surface of the annular zinc oxide ceramic body in a screen printing mode;
thirdly, sintering the product obtained in the second step at high temperature to form a pressure-sensitive junction on the surfaces of the bismuth oxide and zinc oxide ceramic bodies;
step four, placing the product prepared in the third step into vacuum sputtering coating equipment and shielding the position of a polar opening of the annular piezoresistor, firstly sputtering a nickel-chromium alloy transition layer of 1.8-2.3 microns by using nickel-chromium alloy, and then sputtering a copper electrode of 2.8-3.3 microns by using metal copper;
when the step four is executed, the annular piezoresistor is placed in vacuum sputtering coating equipment through a coating supporting plate, the upper surface of the coating supporting plate is covered with a shielding piece, and the shielding piece is used for shielding the position of a pole opening of the annular piezoresistor;
the coating supporting plate is provided with a plurality of circular accommodating grooves corresponding to the annular piezoresistors, and the centers of the accommodating grooves are provided with limiting bulges corresponding to the center holes of the annular piezoresistors.
2. The method for preparing the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material according to claim 1, wherein in the fourth step, the thickness of the nickel-chromium alloy transition layer is 2 microns.
3. The method for preparing the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material according to claim 1, wherein in the fourth step, the thickness of the copper electrode is 3 microns.
4. The method for preparing the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material according to claim 1, wherein the specific process of the third step is as follows: and (3) sintering the product prepared in the step (II) by adopting a mesh belt resistance furnace, wherein the sintering temperature is as follows in sequence: heating at 300 deg.C for 10 min, 500 deg.C for 10 min, 700 deg.C for 10 min, and 850 deg.C for 10 min.
5. The method for preparing the zinc oxide annular piezoresistor vacuum sputtering copper electrode according to the claim 1, wherein in the second step, the annular piezoresistor is placed on the printing table of the screen printing machine through the printing pallet.
6. The method for preparing the annular piezoresistor vacuum sputtering copper electrode made of zinc oxide material according to claim 5, wherein the printing supporting plate is provided with a plurality of circular accommodating grooves corresponding to the annular piezoresistor, the centers of the accommodating grooves are provided with limiting protrusions corresponding to the center holes of the annular piezoresistor, and the circular grooves are provided with 2-4 through holes on the bottom surfaces of the peripheries of the limiting protrusions.
7. The method for preparing the annular piezoresistor vacuum sputtering copper electrode made of the zinc oxide material according to claim 1, wherein in the second step, a 300-mesh screen printing bismuth oxide slurry is adopted, and the thickness of the printing is 5-8 microns.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3723175A (en) * | 1967-10-09 | 1973-03-27 | Matsushita Electric Ind Co Ltd | Nonlinear resistors of bulk type |
| US5004573A (en) * | 1989-11-02 | 1991-04-02 | Korea Institute Of Science And Technology | Fabrication method for high voltage zinc oxide varistor |
| CN102800452A (en) * | 2012-08-29 | 2012-11-28 | 江苏金雷凯光电科技有限责任公司 | Aqueous gel tape casting method for preparing DC (direct current) zinc oxide voltage-sensitive resistor disk |
| CN104576041A (en) * | 2013-10-11 | 2015-04-29 | 邱耀弘 | Substrate with composite electrode layer for large single-layer ceramic passive element |
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2019
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3723175A (en) * | 1967-10-09 | 1973-03-27 | Matsushita Electric Ind Co Ltd | Nonlinear resistors of bulk type |
| US5004573A (en) * | 1989-11-02 | 1991-04-02 | Korea Institute Of Science And Technology | Fabrication method for high voltage zinc oxide varistor |
| CN102800452A (en) * | 2012-08-29 | 2012-11-28 | 江苏金雷凯光电科技有限责任公司 | Aqueous gel tape casting method for preparing DC (direct current) zinc oxide voltage-sensitive resistor disk |
| CN104576041A (en) * | 2013-10-11 | 2015-04-29 | 邱耀弘 | Substrate with composite electrode layer for large single-layer ceramic passive element |
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