CN113314286A - High-strength piezoresistor and preparation method thereof - Google Patents

High-strength piezoresistor and preparation method thereof Download PDF

Info

Publication number
CN113314286A
CN113314286A CN202110593529.9A CN202110593529A CN113314286A CN 113314286 A CN113314286 A CN 113314286A CN 202110593529 A CN202110593529 A CN 202110593529A CN 113314286 A CN113314286 A CN 113314286A
Authority
CN
China
Prior art keywords
electrode layer
chromium
zinc oxide
target
oxide ceramic
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.)
Granted
Application number
CN202110593529.9A
Other languages
Chinese (zh)
Other versions
CN113314286B (en
Inventor
张琪
石国能
岳涛
冯志巍
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Tejet Lightning Protection Technology Co ltd
Original Assignee
Changzhou Tejet Lightning Protection Technology Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Changzhou Tejet Lightning Protection Technology Co ltd filed Critical Changzhou Tejet Lightning Protection Technology Co ltd
Priority to CN202110593529.9A priority Critical patent/CN113314286B/en
Publication of CN113314286A publication Critical patent/CN113314286A/en
Application granted granted Critical
Publication of CN113314286B publication Critical patent/CN113314286B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-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
    • H01C7/10Non-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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C1/00Details
    • H01C1/14Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors
    • H01C1/142Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors the terminals or tapping points being coated on the resistive element
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/28Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals
    • H01C17/288Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals by thin film techniques
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-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
    • H01C7/10Non-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
    • H01C7/105Varistor cores
    • H01C7/108Metal oxide
    • H01C7/112ZnO type

Landscapes

  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermistors And Varistors (AREA)
  • Physical Vapour Deposition (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)

Abstract

The application relates to the field of resistors, and particularly discloses a high-strength piezoresistor and a preparation method thereof. A high strength varistor includes a substrate layer; the X layers of the cladding electrode layers comprise a chromium electrode layer and a copper-nickel alloy electrode layer which are sequentially and repeatedly stacked and deposited from inside to outside, the cladding electrode layers are arranged on the surface of the base body layer, and the number of layers of the chromium electrode layer and the copper-nickel alloy electrode layer is the same; and the resin coating layer is fixedly coated outside the coating electrode layer. A preparation method of a high-strength piezoresistor comprises the following steps: s1, coating a chromium electrode layer; s2, coating a copper-nickel alloy electrode layer; s3, repeating S1 and S2 to prepare an intermediate; and S4, coating the resin layer. According to the preparation method, the electrode layer and the zinc oxide ceramic matrix are stably combined, and the prepared voltage dependent resistor has the advantage of good safety.

Description

High-strength piezoresistor and preparation method thereof
Technical Field
The present application relates to the field of resistors, and more particularly, to a high strength varistor and a method of making the same.
Background
The piezoresistor is a resistor device with nonlinear volt-ampere characteristics, and mainly plays a role in overvoltage protection in a circuit, and the piezoresistor can be roughly divided into a zinc oxide system, a titanium dioxide system and a silicon carbide system according to different main materials, and the zinc oxide system is more applied. The piezoresistor of the zinc oxide system is generally made by adopting a ceramic process, the internal microstructure of the piezoresistor comprises zinc oxide grains and a grain boundary layer around the grains, the resistivity of the zinc oxide grains is very low, the resistivity of the grain boundary layer is higher, when a potential barrier equivalent to a diode is formed between two grains, a piezoresistor unit is formed between the two grains, one piezoresistor comprises a plurality of piezoresistor units which are connected in series, and the number of the piezoresistor units determines the breakdown voltage of the piezoresistor.
In the process of preparing the pressure-sensitive electrode, the powder is generally mixed, the mixture is fired after being subjected to binder removal to form a matrix, the surface of the matrix is coated with an electrode layer, an insulating layer and the like to prepare the pressure-sensitive electrode, and in the process of preparing the pressure-sensitive electrode, the surface of the matrix is coated with metal slurry and then subjected to heat treatment forming to prepare the conductor with excellent conductive performance.
In view of the above-mentioned related technologies, the inventor believes that, in the process of preparing the coating electrode layer of the piezoresistor, the electrode layer needs to be sputtered on the substrate through a single target, and the electrode layer has a certain thickness requirement, which further causes poor bonding performance between the electrode layer and the substrate, and has the defect that the electrode layer is easily separated from the substrate, which further causes the piezoresistor to fail, i.e., the overvoltage protection effect is not good.
Disclosure of Invention
In order to improve the bonding performance between the electrode layer and the substrate and prolong the service life of the piezoresistor, the application provides the high-strength piezoresistor and the preparation method thereof.
The high-strength piezoresistor and the preparation method thereof adopt the following technical scheme:
in a first aspect, the present application provides a high-strength varistor, which adopts the following technical scheme:
a high strength varistor includes a substrate layer; the X layers of the cladding electrode layers comprise a chromium electrode layer and a copper-nickel alloy electrode layer which are sequentially and repeatedly stacked and deposited from inside to outside, the cladding electrode layers are arranged on the surface of the base body layer, and the number of layers of the chromium electrode layer and the copper-nickel alloy electrode layer is the same; and the resin coating layer is fixedly coated outside the coating electrode layer.
Through adopting above-mentioned technical scheme, adopt and repeatedly pile up deposit chromium electrode layer and copper nickel alloy electrode layer in proper order on the base member layer for the electrode layer reaches the required electrode layer thickness of piezo-resistor comparatively easily, improve and adopt single electrode layer to scribble to the required thickness by force after, lead to the not good defect of bonding property between electrode layer and the base member layer, and then reduce the possibility that takes place the separation between electrode layer and the base member layer, prolong piezo-resistor's life, long-term provide overvoltage protection to the circuit.
In a second aspect, the present application provides a method for manufacturing a high-strength varistor, which adopts the following technical scheme:
a preparation method of a high-strength piezoresistor comprises the following steps: s1, coating the chromium electrode layer: taking a zinc oxide ceramic matrix and a chromium target, placing the zinc oxide ceramic matrix and the chromium target in a vacuum chamber, adjusting the vacuum degree in the vacuum chamber, introducing sputtering gas into the vacuum chamber, pre-sputtering for 10-15min, and then performing sputtering treatment on the zinc oxide ceramic matrix to obtain a primary product; s2, coating a copper-nickel alloy electrode layer: taking the primary product and the copper-nickel alloy target, replacing the chromium target with the copper-nickel alloy target, pre-sputtering for 5-10min, and then sputtering the primary product to obtain a secondary product; s3, repeating the steps S1 and S2 to obtain an intermediate; s4, coating resin layer: and coating the epoxy resin on one side of the intermediate, which is coated with the electrode layer, and fluidizing and curing to obtain the piezoresistor.
By adopting the technical scheme, the sputtering target material is excited by an ion bombardment method by adopting a sputtering method, atoms in the target material are further deposited on the surface of the zinc oxide ceramic matrix at a certain speed to form an electrode layer, and the electrode layer prepared by deposition and the zinc oxide ceramic matrix have good bonding performance, so that the electrode layer is attached to the zinc oxide ceramic matrix for a long time, the overvoltage protection effect of the circuit is long-acting and stable, and the safety and the reliability of the piezoresistor are ensured;
meanwhile, the chromium target is sputtered on the zinc oxide ceramic matrix to prepare a primary product, the copper-nickel alloy target is sputtered on the primary product again, circulation is carried out, the multilayer composite electrode layer of chromium-copper-nickel alloy-chromium-copper-nickel alloy is formed on the zinc oxide ceramic matrix, the thickness of the electrode layer required by the piezoresistor is easily achieved, and due to the fact that the speeds of the chromium target and the copper-nickel alloy target impacting the zinc oxide ceramic matrix under the same sputtering pressure are different, the formed electrode layers are combined tightly, the electrode layer and the zinc oxide ceramic matrix are not prone to falling off, the prepared piezoresistor is not prone to failure, and the service life of the piezoresistor is prolonged.
Preferably, the chromium target is prepared by the following method: s1, pressing: placing the target material powder into a pressing mould, pressing and forming, and waiting for static pressure forming to obtain a chromium target ring; s2, sintering treatment: and placing the chromium target ring in a vacuum carbon tube furnace, and sintering by adjusting the sintering temperature to obtain the chromium target.
By adopting the technical scheme, the chromium target ring is prepared by adopting a cold isostatic pressing mode, so that the chromium target ring has better density, the production mode of the cold isostatic pressing reduces the cost, and the economic benefit is improved; by adjusting the sintering temperature, the stress generated by sintering between the chromium target rings can be effectively reduced, and the chromium target with a compact structure is prepared.
Preferably, the temperature change of the sintering treatment is: the temperature is programmed to 300-500 ℃ within 1 h; then the temperature is programmed to 600-800 ℃ within 3 h; introducing argon, and carrying out temperature programming to 1100-1200 ℃ within 7h under the argon atmosphere; finally, the temperature is programmed to 1250 ℃, and the heat preservation treatment is carried out for 1-2 h.
By adopting the technical scheme, the sintering temperature is regulated in stages, so that the stress generated between chromium atoms gradually disappears in the sintering process, and the shrinkage effect of the chromium target ring in the sintering process is better through the improvement of the vacuum degree and the introduction of inert gas, so that the formed chromium target has better density;
and secondly, slowly raising the temperature in the temperature raising process, so that the chromium target ring is uniformly shrunk, and the possibility of deformation or crack of the prepared chromium target is reduced, therefore, the chromium target prepared by the sputtering method can form a uniform chromium electrode layer on the zinc oxide ceramic matrix, and the chromium electrode layer and the zinc oxide ceramic matrix obtain a relatively excellent combination effect.
Preferably, the target powder comprises chromium powder and anhydrous potassium carbonate, and is prepared by the following method: (1) mixing chromium powder and anhydrous potassium carbonate according to the mass ratio of 10-20:1 to prepare mixed powder; (2) and adding the prepared mixed powder into a grinding machine, and grinding for 3 hours to obtain target material powder.
By adopting the technical scheme, a small amount of anhydrous potassium carbonate is added into the chromium powder as a pore forming agent, the surface of the chromium target prepared by adopting the target powder added with the anhydrous potassium carbonate is provided with a small amount of micropores, the surface area of the chromium electrode layer formed on the zinc oxide ceramic matrix by bombarding the chromium target is increased, and the copper-nickel alloy target is continuously sputtered on the primary product, so that the bonding performance between the copper-nickel alloy target and the primary product formed on the zinc oxide ceramic matrix is improved, and the adhesion performance between the electrode layer and the zinc oxide ceramic matrix is further enhanced, therefore, the prepared piezoresistor obtains a lasting overvoltage protection effect on a circuit.
Preferably, the compression molding adopts a bidirectional compression method.
By adopting the technical scheme, the density of the chromium target ring after compression molding is uniform due to the adoption of the bidirectional compression method, the operation method is simple and convenient, and the operation is simple, so that the prepared chromium target ring has better uniformity and compactness.
Preferably, the step S2 of coating the copper-nickel alloy electrode layer further includes the steps of: (1) placing the secondary product in an annealing chamber, adjusting the vacuum degree of the annealing chamber, and adjusting the temperature of the annealing chamber to 350 ℃; (2) and (5) annealing for 1h to obtain an annealed secondary product.
By adopting the technical scheme, due to the annealing treatment, the stress generated between the chromium alloy electrode layer and the copper-nickel alloy electrode layer formed on the zinc oxide ceramic substrate is further eliminated, and the adhesive force between the chromium alloy electrode layer and the copper-nickel alloy electrode layer is improved.
Preferably, before the primary product is coated with the chromium electrode layer in step S2, the pretreatment of the primary product includes the following steps: (1) adjusting the vacuum degree in the vacuum chamber; (2) the primary product is heated to 350-450 ℃ over 2h to obtain the pretreated primary product.
By adopting the technical scheme, as the primary product is subjected to heating pretreatment, the adhesion property between the primary product and the copper-nickel alloy electrode layer is enhanced, the toughness of the chromium electrode layer is improved, and the possibility that the chromium electrode layer is broken and further separated from the zinc oxide ceramic matrix is reduced;
meanwhile, before the copper-nickel electrode layer is coated, the adhesion between the chromium electrode layer and the zinc oxide ceramic matrix is further improved by improving the vacuum degree, so that the pretreated primary product has a better combination effect with the copper-nickel alloy electrode layer.
Preferably, the method further comprises the following substrate processing steps: and respectively placing the zinc oxide ceramic matrix in a hydrochloric acid solution with the mass concentration of 1.5% and a sodium hydroxide solution with the mass concentration of 1.5%, soaking for 5s, taking out, washing with deionized water until the washed solution is neutral, and thus obtaining the zinc oxide ceramic matrix treated by the matrix.
By adopting the technical scheme, the surface of the zinc oxide ceramic matrix is etched by the hydrochloric acid solution and the sodium hydroxide solution, so that the surface area of the zinc oxide ceramic matrix is increased, and the firmness of the combination between the zinc oxide ceramic matrix and the electrode layer is improved, therefore, the prepared piezoresistor is not easy to lose efficacy due to the separation of the electrode layer and the zinc oxide ceramic matrix, and the overvoltage protection can be carried out on a circuit for a long time.
Preferably, the sputtering gas comprises oxygen and argon combined in a volume ratio of 1-4: 100.
By adopting the technical scheme, a small amount of oxygen is mixed in the argon gas, so that the number of atoms participating in the sputtering process of the sputtering target material is increased in the sputtering process, the sputtering speed and the deposition speed of the target material are further increased, the thickness of the prepared electrode layer is uniform, proper resistivity is obtained, and the possibility of separation of the electrode layer and the zinc oxide ceramic matrix is reduced due to the uniform thickness of the motor layer, namely the piezoresistor obtains good reliability.
In summary, the present application has the following beneficial effects:
1. because the chromium electrode layer and the copper-nickel alloy electrode layer are sequentially stacked on the substrate layer, the electrode layer can easily reach the thickness of the electrode layer required by the piezoresistor, and the electrode layer is not easy to be coated to the required thickness by force, so that the adhesion performance between the electrode layer and the substrate layer is poor;
2. the sputtering target is coated on the zinc oxide ceramic matrix to form the electrode layer by adopting a sputtering method, and the sputtering method bombards the sputtering target into atoms which are deposited and attached on the surface of the zinc oxide ceramic matrix at a certain speed, so that the electrode layer and the zinc oxide ceramic matrix have better bonding performance; because the electrode layer is formed by adopting a chromium-copper-nickel alloy-chromium-copper-nickel alloy multilayer metal composite mode, under the same sputtering pressure, the speed of impacting the zinc oxide ceramic matrix is different, so that the electrode layer can impact the zinc oxide ceramic matrix for multiple times, and better adhesion effects are obtained between the electrode layer and the zinc oxide ceramic matrix and between the chromium electrode layer and the copper-nickel alloy electrode layer, namely the prepared piezoresistor has more excellent safety and reliability;
3. the zinc oxide ceramic matrix is preferably subjected to pretreatment, the surface area of the zinc oxide ceramic matrix is increased due to the fact that the zinc oxide ceramic matrix is subjected to etching treatment through a hydrochloric acid solution and a sodium hydroxide solution, and then when a sputtering target material is sputtered on the zinc oxide ceramic matrix to form an electrode layer, the bonding performance between the electrode layer and the zinc oxide ceramic matrix is improved, and the prepared piezoresistor obtains a long-acting circuit overvoltage protection effect.
Detailed Description
The present application will be described in further detail with reference to examples.
In the embodiment of the present application, the selected apparatuses are as follows, but not limited thereto:
the instrument comprises the following steps: the system comprises a JGP-450a type double-chamber magnetron sputtering deposition system, an SX2 type box sintering furnace, a high-temperature vacuum carbonization furnace of Guangchang Gichang technology Limited company, an ST-M200 type high-flux vibration ball mill of Beijing Xuxin Shengke instrument equipment Limited company, a UV-VIS type film thickness measuring instrument of Beijing Purui micro-nano technology Limited company, and a KDY-1 four-probe resistivity measuring instrument of Changzhou Dedu precision instrument Limited company.
Medicine preparation: zinc oxide ceramic substrate of Changxain kang new materials Co., Ltd, an etchant of 2040R2 from Baobang chemical (Shanghai) Co., Ltd, E51128 type epoxy resin from Shandong Kepler Biotechnology Co., Ltd, and a copper-nickel alloy target of Changxin kang new materials Co., Ltd.
Preparation example
Examples of preparation of target powder
Preparation example 1
Firstly, respectively weighing 10kg of chromium powder and 1kg of anhydrous potassium carbonate, mixing to obtain mixed powder, and then placing the prepared mixed powder into a grinding machine to grind for 3 hours to obtain the target material powder 1.
Preparation example 2
Firstly, respectively weighing 15kg of chromium powder and 1kg of anhydrous potassium carbonate, mixing to obtain mixed powder, and placing the mixed powder into a grinding machine to grind for 3 hours to obtain target material powder 2.
Preparation example 3
Firstly, respectively weighing 20kg of chromium powder and 1kg of anhydrous potassium carbonate, mixing to obtain mixed powder, placing the mixed powder in a grinding machine, and grinding for 3 hours to obtain target material powder 3.
Preparation example of chromium target
Preparation example 4
Pressing: firstly, placing target material powder 1 in a pressing mould, pressing and forming in a 300t hydraulic press, and waiting for static pressure forming to obtain a chromium target ring 1;
sintering treatment: then the prepared chromium target ring 1 is placed in a vacuum carbon tube furnace for sintering to prepare a chromium target material 1; the temperature change of the sintering treatment is as follows: firstly, under the vacuum condition, the temperature is programmed to 300 ℃ within 1 h; the vacuum degree is improved, and the temperature is programmed to 600 ℃ within 3 h; introducing argon, and carrying out programmed temperature rise to 1100 ℃ within 7h under the argon atmosphere; finally, the temperature is programmed to 1250 ℃, and the heat preservation treatment is carried out for 1 h.
Preparation example 5
In comparison with preparation example 4, in preparation example 5, the target powder 2 was used in place of the target powder 1 in preparation example 4 to prepare the chromium target 2, and the remaining preparation conditions and steps were the same as in preparation example 4.
Preparation example 6
In comparison with preparation example 4, in preparation example 6, a chromium target 3 was prepared using the target powder 3 in place of the target powder 1 in preparation example 4, and the remaining preparation conditions and steps were the same as in preparation example 4.
Performance test
(1) And (3) testing the density: detecting the chromium target according to GB/T3850-1983 Density determination method of dense sintered metal material and hard alloy, wherein rho is density ratio, and rho = rhoFruit of Chinese wolfberry0×100,ρ0=7.2g/cm3 for the theoretical density of the chromium target;
(2) and (3) detecting the resistivity performance: and detecting the chromium target by adopting a four-pin detector according to GB/T5167-2018 determination of resistivity of sintered metal materials and hard alloys.
TABLE 1 PREPARATION EXAMPLES 4-6 PERFORMANCE TESTS
Figure DEST_PATH_IMAGE001
The comparison of the performance tests in combination with table 1 can find that:
in preparation examples 4 to 6, the density, density ratio and resistivity of the prepared chromium target material are all improved according to the adjustment of the chromium powder and the anhydrous potassium carbonate, which indicates that in this embodiment, the chromium target material is prepared by blending the anhydrous potassium carbonate and the chromium powder, and the resistivity of the chromium target material is improved, because the anhydrous potassium carbonate is evaporated after sintering, micropores are formed on the surface of the chromium target ring, the surface area of the chromium target ring is increased, and the adhesion effect of the electrode layer on the ceramic oxidation substrate is improved, as can be seen from table 1, the chromium target material 3 prepared in preparation example 3 has better resistivity and density, which indicates that the ratio of the chromium powder and the anhydrous potassium carbonate in the target material powder is more appropriate at this time.
Preparation example 7
Pressing: firstly, placing target material powder 3 in a pressing mould, pressing and forming in a 300t hydraulic press, and waiting for static pressure forming to obtain a chromium target ring 4;
sintering treatment: then the prepared chromium target ring 4 is placed in a vacuum carbon tube furnace for sintering to prepare a chromium target 4; the temperature change of the sintering is as follows: firstly, under the vacuum condition, the temperature is programmed to 400 ℃ within 1 h; increasing the vacuum degree, and continuously raising the temperature to 700 ℃ within 3 h; introducing argon, and carrying out programmed temperature rise to 1150 ℃ within 7h under the argon atmosphere; finally, the temperature is programmed to 1250 ℃, and the heat preservation treatment is carried out for 1 h.
Preparation example 8
Pressing: firstly, placing target material powder 3 in a pressing mould, pressing and forming in a 300t hydraulic press, and waiting for static pressure forming to obtain a chromium target ring 5;
sintering treatment: then the prepared chromium target ring 5 is placed in a vacuum carbon tube furnace for sintering to prepare a chromium target 5; the temperature change of the sintering treatment is as follows: firstly, under the vacuum condition, the temperature is programmed to 500 ℃ within 1 h; increasing the vacuum degree, and continuously raising the temperature to 800 ℃ within 3 h; introducing argon, and carrying out programmed temperature rise to 1200 ℃ within 7h under the argon atmosphere; finally, the temperature is programmed to 1250 ℃, and the heat preservation treatment is carried out for 1 h.
Performance test
(1) And (3) testing the density: detecting the chromium target according to GB/T3850-1983 Density determination method of dense sintered metal material and hard alloy, wherein rho is density ratio, and rho = rhoFruit of Chinese wolfberry0×100,ρ0=7.2g/cm3 for the theoretical density of the chromium target;
(2) and (3) detecting the resistivity performance: and detecting the chromium target by adopting a four-pin detector according to GB/T5167-2018 determination of resistivity of sintered metal materials and hard alloys.
TABLE 2 EXAMPLES 7 and 8 Properties examination
Figure 884030DEST_PATH_IMAGE002
The comparison of the performance tests in combination with table 2 can find that:
in preparation examples 7 to 8, the density, density ratio and resistivity of the prepared chromium target material are all improved according to the adjustment of the sintering temperature, which indicates that the chromium target material prepared by sintering the chromium target ring by using the stepped temperature has better density and resistivity, and as can be seen from table 2, the chromium target material 4 prepared in preparation example 7 has better density and resistivity, which indicates that the sintering temperature and the pressing pressure in preparation example 7 are more appropriate at this time.
Preparation examples 9 to 12
Sputtering gases 1, 2, and 3 were prepared by mixing oxygen and argon at volume ratios of 1:100, 2:100, and 4:100, respectively.
Preparation example 13
The difference from preparation example 7 is that: the press forming method adopts bidirectional pressing, and the rest preparation conditions and steps for preparing the chromium target 6 are the same as those of the preparation example 7.
Performance test
(1) And (3) testing the density: detecting the chromium target according to GB/T3850-1983 Density determination method of compact sintered metal material and hard alloy, wherein rho = rhoFruit of Chinese wolfberry0×100,ρ0=7.2g/cm3 for the theoretical density of the chromium target;
(2) and (3) detecting the resistivity performance: and detecting the chromium target by adopting a four-pin detector according to GB/T5167-2018 determination of resistivity of sintered metal materials and hard alloys.
TABLE 3 PREPARATION EXAMPLE 13 Performance test
Figure DEST_PATH_IMAGE003
The comparison of the performance tests in combination with table 3 can find that:
the pressing method is adjusted in the preparation example 13, so that the density and density ratio of the prepared chromium target material are both improved, and the resistivity is increased, which indicates that the chromium target material prepared by the bidirectional pressing method has better uniformity, the compactness of the chromium target material is further enhanced, the surface area of the chromium target ring is reduced, the conductivity of the chromium target material is reduced, and the resistivity is improved due to the compact structure of the chromium target ring, so that the finally prepared chromium target material has better density and resistivity.
Examples
Example 1
Preparing raw materials: firstly, taking a zinc oxide ceramic matrix, a sputtering target material and epoxy resin, wherein the sputtering target material comprises a chromium target material and a copper-nickel alloy target material;
coating an electrode layer: firstly, fixing the zinc oxide ceramic matrix and the sputtering target on a sample table of a vacuum chamber, and enabling the sputtering target to be on a corresponding target position of the vacuum chamber; closing the vacuum chamber, opening circulating water, starting the mechanical pump to low vacuum, and starting the molecular pump until the vacuum degree in the vacuum chamber reaches 3 × 10-2Pa; introducing sputtering gas 1 into the vacuum chamber, carrying out pre-sputtering on the chromium target 4 for 10min, opening a target baffle at 350V, and depositing the chromium target 4 on a zinc oxide ceramic matrix to form a chromium electrode layer to obtain a primary product; shielding the target baffle again, transferring the target pair for pre-sputtering for 5min, adjusting the working air pressure, opening the target baffle, and depositing the copper-nickel alloy target material on the surface of the primary product to form a copper-nickel alloy electrode layer to obtain a secondary product; repeatedly sputtering a chromium electrode layer and a copper-nickel alloy electrode layer, wherein the chromium electrode layer and the copper-nickel alloy electrode layer are both two layers, so as to prepare an intermediate 1;
coating a resin layer: and coating the epoxy resin on one side of the intermediate 1 coated with the electrode layer, and fluidizing and curing to obtain the piezoresistor.
Example 2
The difference from embodiment 1 is that the electrode layer is coated: firstly, fixing the zinc oxide ceramic matrix and the sputtering target on a sample table of a vacuum chamber, and enabling the sputtering target to be on a corresponding target position of the vacuum chamber; closing the vacuum chamber, opening circulating water, starting the mechanical pump to low vacuum, and starting the molecular pump until the vacuum degree in the vacuum chamber reaches 3 × 10-2Pa; introducing sputtering gas 1 into the vacuum chamber, carrying out pre-sputtering on the chromium target 4 for 12min, opening a target baffle at 350V, and depositing the chromium target 4 on a zinc oxide ceramic matrix to form a chromium electrode layer to obtain a primary product; shielding the target baffle again, transferring the target pair for pre-sputtering for 8min, and adjustingAfter the working air pressure is reduced, opening a target baffle plate, depositing the copper-nickel alloy target material on the surface of the primary product to form a copper-nickel alloy electrode layer, and preparing a secondary product; repeatedly sputtering a chromium electrode layer and a copper-nickel alloy electrode layer to prepare an intermediate 2; the varistor was prepared in place of the intermediate 1 in example 1, and the preparation environment and preparation conditions were the same as those in example 1.
Example 3
The difference from embodiment 1 is that the electrode layer is coated: firstly, fixing the zinc oxide ceramic matrix and the sputtering target on a sample table of a vacuum chamber, and enabling the sputtering target to be on a corresponding target position of the vacuum chamber; closing the vacuum chamber, opening circulating water, starting the mechanical pump to low vacuum, and starting the molecular pump until the vacuum degree in the vacuum chamber reaches 3 × 10-2Pa; introducing sputtering gas 1 into the vacuum chamber, carrying out pre-sputtering on the chromium target 4 for 15min, opening a target baffle at 350V, and depositing the chromium target 4 on a zinc oxide ceramic matrix to form a chromium electrode layer to obtain a primary product; shielding the target baffle again, transferring the target pair for pre-sputtering for 10min, adjusting the working air pressure, opening the target baffle, depositing the copper-nickel alloy target material on the surface of the primary product to form a copper-nickel alloy electrode layer, and preparing a secondary product; repeatedly sputtering a chromium electrode layer and a copper-nickel alloy electrode layer to prepare an intermediate 3; the varistor was prepared in place of the intermediate 1 in example 1, and the preparation environment and preparation conditions were the same as those in example 1.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter; detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: detecting the adhesive force between the electrode layer and the zinc oxide ceramic matrix by adopting a tension meter with the model of XLW (PC) -500N;
(4) and (3) detection of tolerance current capacity: applying 8 mus/20 mus shock wave of peak current 3kA to test the resistance of piezoresistor to current, measuring the piezoresistor before and after impactRatio of pressures V0
Table 4 examples 1-3 performance testing
Figure 456962DEST_PATH_IMAGE004
The comparison of the performance tests in combination with table 4 can find that:
in the embodiments 1 to 3, the pre-sputtering time is adjusted, so that the leakage current and the voltage of the manufactured varistor are reduced, and the tensile strength is improved, which indicates that the application adopts the pre-sputtering for a certain time before the sputtering, so that the electrode layer sputtered and deposited on the zinc oxide ceramic substrate is relatively uniform and has a suitable vacuum degree, so that the sputtering speed of the target material is relatively good, and the bonding capability of the electrode layer and the zinc oxide ceramic substrate is improved.
Example 4
The difference from example 2 is that: in example 4, a varistor was produced using the sputtering gas 2 in place of the sputtering gas 1 in example 2, and the production environment and production conditions were the same as those in example 2.
Example 5
The difference from example 2 is that: in example 5, a varistor was produced using sputtering gas 3 in place of sputtering gas 1 in example 2, and the production environment and production conditions were the same as in example 2.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: detecting the adhesive force between the electrode layer and the zinc oxide ceramic matrix by adopting a tension meter with the model of XLW (PC) -500N;
(4) and (3) detection of tolerance current capacity: the 8 mu s/20 mu s shock wave with peak current of 3kA is applied to test the current endurance capacity of the piezoresistor, and the ratio V of the voltage before and after the shock is measured0
Table 5 examples 4-5 performance testing
Figure DEST_PATH_IMAGE005
The comparison of the performance tests in combination with table 4 can find that:
in examples 4 to 5, the sputtering gas was adjusted to reduce the leakage current and the varistor voltage of the varistor, and the tensile strength was improved, the method adopts the argon and the oxygen to prepare the sputtering gas, improves the number of atoms generated by the sputtering target material in bombardment, promotes the sputtering target material to deposit on the zinc oxide ceramic matrix, obtains an electrode layer with uniform deposition on the zinc oxide ceramic matrix, reduces the possibility that the electrode layer is easy to separate from the zinc oxide ceramic matrix due to uneven thickness of the electrode layer, ensures that the piezoresistor can carry out overvoltage protection on the circuit for a long time, as can be seen from table 4, the varistor prepared in example 2 has a higher varistor voltage and a smaller leakage current, and a better tensile strength, which indicates that the ratio of argon to oxygen in the sputtering gas in preparative example 4 is suitable.
Example 6
The difference from example 4 is that: in example 6, a chromium target 6 was used instead of the chromium target 4 in example 4 to prepare a varistor, and the rest of the preparation environment and the preparation conditions were the same as those in example 4.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: detecting the adhesive force between the electrode layer and the zinc oxide ceramic matrix by adopting a tension meter with the model of XLW (PC) -500N;
(4) and (3) detection of tolerance current capacity: the 8 mu s/20 mu s shock wave with peak current of 3kA is applied to test the current endurance capacity of the piezoresistor, and the ratio V of the voltage before and after the shock is measured0
Table 6 example 6 performance testing
Figure 643224DEST_PATH_IMAGE006
In combination with the comparison of the performance tests in table 6, it can be found that:
in embodiment 6, the pressing method is adjusted, and the electrode thickness and the tensile strength of the prepared varistor are both improved, which indicates that the chromium target prepared by the bidirectional pressing method has better density and uniformity, and then the electrode layer formed on the zinc oxide ceramic matrix by sputtering the chromium target has better uniformity, so that the bonding performance between the electrode layer and the zinc oxide ceramic matrix is improved, the electrode layer is not easily separated from the zinc oxide ceramic matrix, and the prepared varistor has better safety.
Example 7
The difference from example 6 is that the zinc oxide ceramic substrate is prepared by surface treatment of a finished substrate before being placed in a vacuum chamber, and comprises the following steps: the zinc oxide ceramic matrix is respectively placed in a hydrochloric acid solution with the mass concentration of 1.5% and a sodium hydroxide solution with the mass concentration of 1.5%, soaked for 5 seconds, taken out, washed by deionized water until the washed solution is neutral, and the zinc oxide ceramic matrix treated by the matrix is prepared to replace the zinc oxide ceramic matrix in the example 6 to prepare the piezoresistor, wherein the rest preparation environments and preparation conditions are the same as those in the example 6.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: detecting the adhesive force between the electrode layer and the zinc oxide ceramic matrix by adopting a tension meter with the model of XLW (PC) -500N;
(4) and (3) detection of tolerance current capacity: the 8 mu s/20 mu s shock wave with peak current of 3kA is applied to test the current endurance capacity of the piezoresistor, and the ratio V of the voltage before and after the shock is measured0
Table 7 example 7 performance testing
Figure DEST_PATH_IMAGE007
In combination with the comparison of the performance tests in table 7, it can be found that:
in embodiment 7, the surface treatment is performed on the zinc oxide ceramic substrate, and the adhesion and thickness of the prepared varistor are increased, which indicates that the surface treatment is performed on the zinc oxide ceramic substrate in the present application, so that the adhesion between the electrode layer and the zinc oxide ceramic substrate on the prepared varistor can be effectively improved.
Example 8
The difference from example 7 is that the primary product is pretreated before the formation of the intermediate substrate, comprising the following steps: firstly, the vacuum degree in the vacuum chamber is adjusted to 10-2Pa, and the primary product was heated to 350 ℃ over 2 hours to obtain a pretreated primary product, and a varistor was prepared in place of the varistor of example 7, and the remaining preparation conditions and conditions were the same as those of example 7.
Example 9
The difference from example 7 is that a varistor was prepared by heating the primary product to 400 ℃ over 2 hours, instead of the varistor of example 8, and the preparation environment and preparation conditions were the same as those of example 8.
Example 10
The difference from example 7 is that a varistor was prepared by heating the primary product to 450 ℃ over 2 hours, instead of the varistor of example 8, and the preparation environment and preparation conditions were the same as those of example 8.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: the tension meter respectively detects the adhesive forces L1 and L2 between the electrode layer and the zinc oxide ceramic matrix and between the copper-nickel alloy and the primary product;
(4) and (3) detection of tolerance current capacity: the 8 mu s/20 mu s shock wave with peak current of 3kA is applied to test the current endurance capacity of the piezoresistor, and the ratio V of the voltage before and after the shock is measured0
Table 8 examples 8-10 performance testing
Figure 379711DEST_PATH_IMAGE008
In combination with the comparison of the performance tests in table 8, it can be found that:
in examples 8 to 10, the primary product is pretreated to increase the tensile strength between the electrode layer and the zinc oxide ceramic substrate in the varistor and the tensile strength between the copper-nickel alloy electrode layer and the primary product, which means that the pretreatment of the primary product can effectively improve the adhesion between the copper-nickel alloy electrode layer and the chromium electrode layer in the varistor, thereby reducing the thickness of the electrode layer, increasing the bonding between the electrode layer and the zinc oxide ceramic substrate, i.e., reducing the possibility of damage to the varistor, and prolonging the service life of the varistor, as can be seen from table 8, the electrode layer and the zinc oxide ceramic substrate in the varistor prepared in example 10 have strong adhesion, which means that the temperature of the primary product is increased in example 10 appropriately.
Example 11
The difference from example 10 is that the secondary product is prepared by the following method: sputtering a primary product to prepare an intermediate substrate by using a copper-nickel alloy target material at 350V; placing the prepared intermediate substrate in an annealing chamber with vacuum degree of 6 × 10-2Pa, and annealing at 350 deg.C for 1h to obtain a secondary product, instead of the secondary product in example 10, to prepare a varistor, and the rest of the preparation environment and preparation conditions were the same as those in example 10.
Example 12
The difference from example 11 is that the chromium electrode layer and the copper-nickel alloy electrode layer are three layers, and the rest of the preparation environment and the preparation conditions are the same as those in example 11.
Example 13
The difference from example 11 is that the chromium electrode layer and the copper-nickel alloy electrode layer are four layers, and the rest of the preparation environment and the preparation conditions are the same as those in example 11.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: the tension meter respectively detects the adhesive forces L1 and L2 between the electrode layer and the zinc oxide ceramic matrix and between the copper-nickel alloy and the primary product;
(4) and (3) detection of tolerance current capacity: the 8 mu s/20 mu s shock wave with peak current of 3kA is applied to test the current endurance capacity of the piezoresistor, and the ratio V of the voltage before and after the shock is measured0
TABLE 9 EXAMPLES 11-13 Performance testing
Figure DEST_PATH_IMAGE009
Referring to the comparison of the performance tests in tables 8 and 9, it can be found that:
(1) in example 11, the pressure in the vacuum chamber is adjusted, and the secondary product is annealed to obtain the piezoresistor in which the tensile strength between the electrode layer and the zinc oxide ceramic substrate and the tensile strength between the copper-nickel alloy electrode layer and the primary product are both significantly improved, which indicates that the application can improve the sputtering speed of the copper-nickel alloy target by adjusting the pressure in the vacuum chamber, so that when the bombarded atoms are deposited on the primary product, the bombarded atoms have a certain acceleration, thereby improving the bonding performance between the chromium electrode layer and the zinc oxide ceramic substrate, and simultaneously improving the bonding performance between the copper-nickel alloy electrode layer and the primary product, and thus effectively improving the adhesion between the electrode layer and the zinc oxide ceramic substrate; and secondly, through annealing treatment, the bonding effect between the copper-nickel alloy electrode layer and the chromium electrode layer is further improved, the prepared piezoresistor is not easy to lose efficacy due to the falling of the electrode layer and the zinc oxide ceramic substrate, and the service life of the piezoresistor is prolonged.
(2) Comparing examples 12-13 with example 11, it can be found that adjusting the number of the chromium electrode layer and the copper nickel alloy electrode layer, the tensile strength between the electrode layer of the prepared varistor and the zinc oxide ceramic substrate is improved, and the tensile strength between the copper nickel alloy electrode layer and the primary product is significantly improved, which indicates that the multilayer composite electrode layer of chromium-copper nickel alloy-chromium-copper nickel alloy is formed on the zinc oxide ceramic substrate in the present application, so as to effectively improve the tensile strength between the electrode layer and the zinc oxide ceramic substrate, because of the multilayer composite structure, not only the electrode layer can easily reach the thickness required by the varistor electrode layer, but also in the sputtering process, because the chromium target and the copper nickel alloy target impact the zinc oxide ceramic substrate at the same sputtering pressure at different speeds, so that each prepared electrode layer has excellent bonding performance, therefore, the bonding effect between the electrode layer and the zinc oxide ceramic substrate is improved, and the service life of the varistor is prolonged, as can be seen from table 9, the bonding performance between the electrode layer and the zinc oxide ceramic substrate on the varistor manufactured in example 12 is better, which indicates that the chromium electrode layer and the copper-nickel alloy electrode layer are both three layers better.
Comparative example
Comparative example 1
Pure argon gas was used to prepare a sputtering gas instead of the sputtering gas used in example 12 to prepare a varistor, and the remaining preparation conditions and the preparation environment were the same as those of example 12.
Comparative example 2
The chromium target ring is placed in a vacuum carbon tube furnace, and is heated to 1200 ℃ by a program under vacuum, and is sintered for 10 hours under heat preservation to prepare the chromium target material, so as to replace the chromium target material in the embodiment 12, prepare the piezoresistor, and the rest preparation environment and preparation conditions are the same as those in the embodiment 12.
Comparative example 3
The finished substrate was subjected to surface treatment with a commercially available surface etching treatment agent to prepare a zinc oxide ceramic substrate in place of the zinc oxide ceramic substrate in example 12 to prepare a varistor, and the remaining preparation conditions and preparation conditions were the same as those in example 12.
Comparative example 4
The copper-nickel alloy target is sputtered at 500V to obtain an intermediate substrate instead of the intermediate substrate in example 12, and the varistor is prepared under the same preparation environment and conditions as those in example 12.
Comparative example 5
The intermediate substrate in example 12 was replaced by a copper-nickel alloy target at 200V, and the primary product was sputtered to prepare an intermediate substrate, and the remaining preparation environment and preparation conditions were the same as those in example 12.
Performance test
(1) Measuring the voltage-sensitive voltage, nonlinear coefficient and leakage current parameters of the piezoresistor by adopting a voltage-sensitive three-parameter tester with the model of MOVTTK-168;
(2) and (3) thickness detection: detecting the thickness of the electrode layer by using a film thickness meter;
(3) and (3) detecting the tensile strength: the tension meter respectively detects the adhesive forces L1 and L2 between the electrode layer and the zinc oxide ceramic matrix and between the copper-nickel alloy and the primary product;
(4) and (3) detection of tolerance current capacity: the 8 mu s/20 mu s shock wave with peak current of 3kA is applied to test the current endurance capacity of the piezoresistor, and the ratio V of the voltage before and after the shock is measured0
TABLE 10 comparative examples 1-5 Performance test
Figure 600608DEST_PATH_IMAGE010
(1) Comparing comparative example 1 with example 12, the adhesion performance of the electrode layer and the zinc oxide ceramic matrix in the varistor prepared in comparative example 1 is reduced, and the thickness of the electrode layer is improved, which shows that the application adopts the mixture of argon and oxygen as the sputtering gas, so that the adhesion performance of the electrode layer and the zinc oxide ceramic matrix on the varistor is improved, because the argon and the oxygen are mixed, the number of atoms sputtered on the sputtering target is increased, meanwhile, the deposition speed of the sputtering target on the zinc oxide ceramic matrix is increased, and further, the coverage rate of the sputtering target on the zinc oxide ceramic matrix is increased, namely, the uniformity of the electrode layer is improved, the possibility of separation of the electrode layer and the zinc oxide ceramic matrix caused by uneven thickness of the electrode layer is reduced, and the timeliness of the varistor for overvoltage protection of the circuit is prolonged.
(2) Comparing comparative example 2 with example 12, the varistor prepared in comparative example 2 has a reduced varistor voltage, an increased leakage current, a significantly reduced adhesion between the electrode layer and the zinc oxide ceramic substrate in the varistor, this shows that the chromium target is sintered by heating stage by stage, the prepared piezoresistor has good performance in all aspects, the electrode layer in the piezoresistor has good bonding performance with the zinc oxide ceramic substrate, this is because the sintering temperature is adjusted in stages so that the stress generated between the chromium atoms gradually disappears during the sintering process, the shrinkage effect of the chromium target ring in the sintering process is better, a uniform chromium target material is formed, the chromium target material is sputtered on a uniform chromium electrode layer formed on the zinc oxide ceramic matrix, the bonding performance between the chromium electrode layer and the zinc oxide ceramic matrix is improved, and the safety and the reliability of the piezoresistor are improved.
(3) Comparing comparative example 3 with example 12, the tensile effect of the electrode layer and the zinc oxide ceramic matrix in the varistor prepared in comparative example 3 is reduced, which shows that the etching effect of the zinc oxide ceramic matrix is improved by adopting the acid etching and alkali etching composite etching, the surface area of the zinc oxide ceramic matrix is uniformly increased, and the bonding effect between the electrode layer and the zinc oxide ceramic matrix is effectively improved.
(4) Comparing comparative examples 4 and 5 with example 12, the adhesion effect of the electrode layer of the varistor prepared in comparative examples 4 and 5 and the zinc oxide ceramic substrate is reduced, because under an excessively high pressure, atoms in the sputtering target material overflow excessively, and the excessive atoms collide during the sputtering process, thereby not only reducing the deposition speed of the sputtering target material on the zinc oxide ceramic substrate, but also reducing the deposition uniformity of the sputtering target material on the zinc oxide ceramic substrate, and further the bonding effect of the electrode layer and the zinc oxide ceramic substrate is poor; too low pressure causes less atoms to overflow from the sputtering target material, so that the uniformity of the formed electrode layer is poor, and the bonding effect of the electrode layer and the zinc oxide ceramic matrix is poor; the application shows that the electrode layer and the zinc oxide ceramic matrix with better bonding performance can be obtained by adopting the proper sputtering pressure and better deposition speed and deposition uniformity of the sputtering target on the zinc oxide ceramic matrix, and the service life of the piezoresistor is prolonged.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (10)

1. A high strength varistor characterized in that: comprises that
A substrate layer;
the X layers of the cladding electrode layers comprise a chromium electrode layer and a copper-nickel alloy electrode layer which are sequentially and repeatedly stacked and deposited from inside to outside, the cladding electrode layers are arranged on the surface of the base body layer, and the number of layers of the chromium electrode layer and the copper-nickel alloy electrode layer is the same;
and the resin coating layer is fixedly coated outside the coating electrode layer.
2. A preparation method of a high-strength piezoresistor is characterized by comprising the following steps:
s1, coating the chromium electrode layer: taking a zinc oxide ceramic matrix and a chromium target, placing the zinc oxide ceramic matrix and the chromium target in a vacuum chamber, adjusting the vacuum degree in the vacuum chamber, introducing sputtering gas into the vacuum chamber, pre-sputtering for 10-15min, and then performing sputtering treatment on the zinc oxide ceramic matrix to obtain a primary product;
s2, coating a copper-nickel alloy electrode layer: taking the primary product and the copper-nickel alloy target, replacing the chromium target with the copper-nickel alloy target, pre-sputtering for 5-10min, and then sputtering the primary product to obtain a secondary product;
s3, repeating the steps S1 and S2 to obtain an intermediate;
s4, coating resin layer: and coating the epoxy resin on one side of the intermediate body coated with the electrode layer, and fluidizing and curing to obtain the piezoresistor.
3. The method for preparing a high-strength piezoresistor according to claim 2, wherein the chromium target is prepared by the following method:
(1) pressing: placing the target material powder into a pressing mould, pressing and forming, and waiting for static pressure forming to obtain a chromium target ring;
(2) sintering treatment: and placing the chromium target ring in a vacuum carbon tube furnace, adjusting the sintering temperature, and sintering to obtain the chromium target.
4. The method for preparing a high-strength piezoresistor according to claim 3, wherein the temperature change of the sintering treatment is as follows: the temperature is programmed to 300-500 ℃ within 1 h; then the temperature is programmed to 600-800 ℃ within 3 h; introducing argon, and carrying out temperature programming to 1100-1200 ℃ within 7h under the argon atmosphere; finally, the temperature is programmed to 1250 ℃, and the heat preservation treatment is carried out for 1-2 h.
5. The method for preparing a high-strength piezoresistor according to claim 3, wherein the target powder comprises chromium powder and anhydrous potassium carbonate, and is prepared by the following method:
(1) mixing chromium powder and anhydrous potassium carbonate according to the mass ratio of 10-20:1 to prepare mixed powder;
(2) and adding the prepared mixed powder into a grinding machine, and grinding for 3 hours to obtain target material powder.
6. The method for preparing a high-strength varistor according to claim 3, characterized in that: the method adopted by the compression molding is a bidirectional compression method.
7. The method according to claim 2, wherein the step S2 of coating the copper-nickel alloy electrode layer further comprises the steps of:
(1) placing the secondary product in an annealing chamber, adjusting the vacuum degree of the annealing chamber, and adjusting the temperature of the annealing chamber to 350 ℃;
(2) and (5) annealing for 1h to obtain an annealed secondary product.
8. The method according to claim 2, wherein the step S2 of pre-treating the primary product before coating the chromium electrode layer with the primary product comprises the following steps:
(1) adjusting the vacuum degree in the vacuum chamber;
(2) the primary product is heated to 350-450 ℃ by the 2h program to obtain the pretreated primary product.
9. The method for preparing a high strength varistor according to claim 1, further comprising a substrate processing step of:
and respectively placing the zinc oxide ceramic matrix in a hydrochloric acid solution with the mass concentration of 1.5% and a sodium hydroxide solution with the mass concentration of 1.5%, soaking for 5s, taking out, washing with deionized water until the washed solution is neutral, and thus obtaining the zinc oxide ceramic matrix treated by the matrix.
10. The method for preparing a high-strength piezoresistor according to claim 2, wherein: the sputtering gas comprises oxygen and argon which are combined according to the volume ratio of 1: 4-100.
CN202110593529.9A 2021-05-28 2021-05-28 High-strength piezoresistor and preparation method thereof Active CN113314286B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110593529.9A CN113314286B (en) 2021-05-28 2021-05-28 High-strength piezoresistor and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110593529.9A CN113314286B (en) 2021-05-28 2021-05-28 High-strength piezoresistor and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113314286A true CN113314286A (en) 2021-08-27
CN113314286B CN113314286B (en) 2022-09-06

Family

ID=77376165

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110593529.9A Active CN113314286B (en) 2021-05-28 2021-05-28 High-strength piezoresistor and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113314286B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102496431A (en) * 2011-12-12 2012-06-13 中国振华集团云科电子有限公司 Manufacturing method of platinum film resistor chip for temperature sensor
CN203617055U (en) * 2013-09-17 2014-05-28 昆山萬豐電子有限公司 Zinc oxide pressure-sensitive resistor with composite electrode structure
CN204257308U (en) * 2014-11-03 2015-04-08 厦门万明电子有限公司 A kind of zinc oxide varistor
CN108922702A (en) * 2018-05-24 2018-11-30 江苏时瑞电子科技有限公司 A kind of electrode production process of zinc oxide varistor
CN111996507A (en) * 2020-08-14 2020-11-27 宁波江丰电子材料股份有限公司 Preparation method of chromium-silicon sputtering target material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102496431A (en) * 2011-12-12 2012-06-13 中国振华集团云科电子有限公司 Manufacturing method of platinum film resistor chip for temperature sensor
CN203617055U (en) * 2013-09-17 2014-05-28 昆山萬豐電子有限公司 Zinc oxide pressure-sensitive resistor with composite electrode structure
CN204257308U (en) * 2014-11-03 2015-04-08 厦门万明电子有限公司 A kind of zinc oxide varistor
CN108922702A (en) * 2018-05-24 2018-11-30 江苏时瑞电子科技有限公司 A kind of electrode production process of zinc oxide varistor
CN111996507A (en) * 2020-08-14 2020-11-27 宁波江丰电子材料股份有限公司 Preparation method of chromium-silicon sputtering target material

Also Published As

Publication number Publication date
CN113314286B (en) 2022-09-06

Similar Documents

Publication Publication Date Title
US9824868B2 (en) Sputtering target and method for producing the same
US20130224422A1 (en) Molybdenum containing targets
JP5203908B2 (en) Ni-Mo alloy sputtering target plate
KR20160099556A (en) W-ni sputter target
US7138350B2 (en) MgO vapor deposition material and method for preparation thereof
KR101955746B1 (en) Sputtering target and method for producing same
TWI244504B (en) Silicon sintered compact and method for producing the same
CN113314286B (en) High-strength piezoresistor and preparation method thereof
US11837449B2 (en) Ti-Nb alloy sputtering target and production method thereof
CN115896726A (en) MAX-Ag phase composite coating and preparation method and application thereof
EP2228805A1 (en) Transparent conducive film and method for producing the same
JP2000129432A (en) Electroconductive metallic oxide sinetred body and its use
CN115354278A (en) Preparation method of thin film resistor in thin film resistance-capacitance network
JP5754093B2 (en) Zinc oxide sintered body, manufacturing method thereof, sputtering target, and manufacturing method of transparent film
CN109338289B (en) Preparation method of carbon/carbon composite material anti-oxidation coating
JP4000813B2 (en) Sputtering target
JP2004059965A (en) Sputtering target and method for manufacturing the same
JP4895481B2 (en) Resistance thin film and sputtering target for forming the resistance thin film
JP2021075749A (en) Sputtering target
CN114150281B (en) Tantalum nitride film and preparation method thereof
JP3852446B2 (en) Resistance thin film material and method of manufacturing resistance thin film using the same
WO2000031316A1 (en) Co-Ti ALLOY SPUTTERING TARGET AND MANUFACTURING METHOD THEREOF
JP4630025B2 (en) Method for producing copper alloy material
JP4042714B2 (en) Metal resistor material, sputtering target and resistive thin film
JP2005294612A5 (en)

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant