CN115149903A - Silver palladium copper crystal oscillator electrode and process - Google Patents
Silver palladium copper crystal oscillator electrode and process Download PDFInfo
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- CN115149903A CN115149903A CN202210749188.4A CN202210749188A CN115149903A CN 115149903 A CN115149903 A CN 115149903A CN 202210749188 A CN202210749188 A CN 202210749188A CN 115149903 A CN115149903 A CN 115149903A
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- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03B—GENERATION OF OSCILLATIONS, DIRECTLY OR BY FREQUENCY-CHANGING, BY CIRCUITS EMPLOYING ACTIVE ELEMENTS WHICH OPERATE IN A NON-SWITCHING MANNER; GENERATION OF NOISE BY SUCH CIRCUITS
- H03B5/00—Generation of oscillations using amplifier with regenerative feedback from output to input
- H03B5/02—Details
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
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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
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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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
Abstract
An electrode of Ag-Pd-Cu crystal oscillator is prepared from Ag, pd, cu, in, fe and Se. The specific contents are 97.65 percent to 98.124 percent of Ag, 0.86 percent to 1.25 percent of Pd, 0.62 percent to 0.94 percent of Cu, 0.42 percent to 0.69 percent of In, 0.20 percent to 0.35 percent of Te and 0.16 percent to 0.28 percent of Se according to the mass ratio. After the silver, palladium and copper alloy materials are adopted as the crystal oscillator electrodes, the stability of frequency is improved during thermal shock; the adopted film coating process is convenient and fast to operate, uniform in film forming, and capable of solving the problem of frequency drift, the adopted annealing process improves the compactness, the uniformity and the high-temperature stability of the crystal grains of the metal film, and can prevent secondary crystallization of the crystal grains, so that the anti-fatigue property of the metal film is improved.
Description
Technical Field
The invention relates to the technical field of production and manufacturing of crystal oscillators, in particular to a silver-palladium-copper crystal oscillator electrode and a process.
Background
The information technology is one of three main pillars for the development of the modern society, and the Internet of things is an important component of the information technology of the new generation. The wireless communication is the key for realizing the wireless transmission of the information of the Internet of things and is an important guarantee for further improving the information consumption scale and benefit. Wireless communication is not separated from a basic component, namely a crystal oscillator (crystal oscillator), to provide a clock with a basic frequency. The quartz crystal oscillator is a resonance device made by using the piezoelectric effect of quartz crystal (crystal of silicon dioxide), and is the heart of wireless communication hardware. The stability in the working temperature is one of the main characteristics of the crystal oscillator, and directly influences the reliability and stability of the whole wireless communication. Crystal aging is another important factor causing frequency variation, and the crystal aging causes the output frequency to vary according to a logarithmic curve, thereby affecting the stability of wireless communication. In recent years, with the continuous upgrading of wireless technology and the continuous improvement and increase of transmission speed and transmission data volume, the requirement on frequency precision is more and more severe. Then, an important problem exists at present, after the crystal oscillator is subjected to a transient environmental change (thermal shock), the frequency of the crystal oscillator generates a large fluctuation, which affects the stability of wireless communication and even causes a disconnection. Analysis shows that the frequency of the crystal is greatly fluctuated after the crystal is subjected to transient environmental change, and the reason is that the metal electrode is oxidized or recrystallized at high temperature, and the conductivity and the quality of the electrode are influenced. The increase in the surface quality of the crystal leads to a shift in frequency.
Although the use of gold as the electrode film can obtain an extremely stable frequency characteristic, the price thereof is tens of times higher than that of silver, and the cost thereof also rises by 20-40%, which causes a large decline in the competitiveness in the market and a failure to gain the market. The quality and the cost become the dilemma of the crystal oscillator industry in the market.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the silver-palladium-copper crystal oscillator electrode and the process, when the electrode is subjected to thermal shock, the frequency is stable, the variation is small, the manufacturing cost is low, and the specific technical scheme is as follows:
the specific components of the silver-palladium-copper crystal oscillator electrode comprise silver, palladium and copper, and form an alloy material.
As an optimization: also includes indium, iron and selenium.
As an optimization: the specific content of Ag is more than or equal to 97.65 percent and less than or equal to 98.124 percent according to the mass ratio,
0.86％≤Pd≤1.25％，0.62％≤Cu≤0.94％，0.42％≤In≤0.69％，0.20％≤Te≤0.35％，0.16％≤Se≤0.28％。
a film coating process for an electrode of a silver palladium copper crystal oscillator comprises the following specific steps:
the method comprises the following steps: cleaning a coating chamber;
step two: preparing a substrate, cleaning a glass slide, and closing a vacuum chamber;
step three: starting a power supply of the vacuum machine, and preheating for 8-15 minutes;
step four: switch-on electron a diffractometer power supply;
step five: keeping the air pressure of the vacuum chamber and the vacuum chamber gas storage bottle to be 5-6.7 Pa;
step six: cooling water is connected, an oil diffusion pump is started, and preheating is carried out for 30-50 minutes;
step seven: after preheating, observing the indication of the vacuum gauge, when the indication is lower than 0.1 Pa, turning on a lamp filament, switching on the ionization gauge, and continuously converting the maximum measuring range until the indication is less than 5 Pa;
step eight: the current is adjusted according to the hot red degree of the tungsten filament when the film coating is started;
step nine: observing the film coating condition, and when the red light of the tungsten filament is shielded, slowly closing the current switch after film coating is finished, and then closing the film coating switch and the film coating baffle;
step ten: closing the high vacuum butterfly valve and cutting off the power supply of the oil diffusion pump;
step eleven: cooling for 5-10 min, closing the mechanical pump, inflating the vacuum chamber, opening the film coating chamber after inflation is finished, taking out the product, and observing the film coating condition;
step twelve: and (6) ending.
A coating annealing process of a silver palladium copper crystal oscillator electrode comprises the following specific steps:
the method comprises the following steps: putting into a coating, increasing the speed of 5-10 ℃ per minute to 700-900 ℃, and keeping for 25-35 minutes;
step two: cooling to 550-650 deg.C, and maintaining for 25-35 min;
step three: heating to 700-750 deg.c and maintaining for 25-35 min;
step four: cooling to 450-550 deg.C, and maintaining for 25-35 min;
step five: heating to 600-650 deg.C, and maintaining for 25-35 min;
step six: cooling to 350-450 deg.C, and maintaining for 25-35 min;
step seven: stopping heating and naturally cooling.
The beneficial effects of the invention are as follows: after the silver-palladium-copper alloy material is used as the crystal oscillator electrode, the stability of frequency during thermal shock is improved; the adopted film coating process is convenient and fast to operate, uniform in film forming, and capable of solving the problem of frequency drift, the adopted annealing process improves the compactness, the uniformity and the high-temperature stability of the crystal grains of the metal film, and can prevent secondary crystallization of the crystal grains, so that the anti-fatigue property of the metal film is improved.
Drawings
FIG. 1 is a diagram showing the crystal change after heating of the electrode according to the present invention.
Fig. 2 is a graph showing the thermal shock resistance of a silver electrode film and a silver palladium copper electrode film according to the present invention.
Fig. 3 is a graph showing aging stability characteristics of the load resonance frequency of the ag electrode film and the ag pd-cu electrode film crystal oscillator according to the present invention.
FIG. 4 is a heat shock resistance test chart of a 7M26M crystal oscillator of a silver electrode film and a silver palladium copper electrode film according to the present invention.
FIG. 5 is a diagram showing the crystal change in heat resistance of the annealing process in the present invention.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
An electrode of silver-palladium-copper crystal oscillator is prepared by adding palladium (Pd), copper (Cu) and other elements into silver to form Ag-palladium-copper (Ag-Pd-Cu: APC) alloy electrode material; the concrete contents are as follows according to mass ratio: ag is between 97.65% and 98.124%, pd is between 0.86% and 1.25%, cu is between 0.62% and 0.94%, in is between 0.42% and 0.69%, te is between 0.20% and 0.35%, se is between 0.16% and 0.28%.
As shown in fig. 1, the grain size of the ag-pd-cu alloy slightly increased with an increase of 325 ℃ in the baking temperature in vacuum. However, the ag-pd-cu alloy can suppress the increase of the grain size and improve the thermal stability, compared with pure ag.
As shown in fig. 2: after the 7M26M crystal oscillator uses the silver palladium copper electrode film, the variation of the frequency of the 7M26M crystal oscillator after thermal shock is less than 1.20ppm, and good frequency stability is shown. Similarly, in the case of a 7M26M crystal oscillator using an Ag film as an electrode, the amount of change in frequency before and after thermal shock was about 3ppm, which was smaller than that of the sample using the silver palladium copper electrode film. The frequency stability of the silver palladium copper electrode film is better than that of an Ag film. The results show that the thermal shock resistance of the silver palladium copper film used as the electrode is greatly improved, and the stability of the Ag film used as the crystal oscillator can be improved.
FIG. 3 shows: aging stability test results for a 7M26M model temperature sensor (HTS) crystal oscillator after using Ag, silver palladium copper electrode films. It can be seen that the 7M26M crystal oscillator using the silver palladium copper electrode film after aging, the variation of the frequency was less than 2ppm, showing good frequency aging stability. Similarly, in the case of a 7M26M crystal oscillator using an Ag film as an electrode, the frequency change amount before and after thermal shock was about 3.5ppm, and the stability was lower than that of the sample using a silver palladium copper electrode film. The frequency stability of the silver palladium copper electrode film is better than that of an Ag film. The result shows that the silver palladium copper alloy film can obviously improve the aging stability of the pure silver film as the electrode of the crystal oscillator.
As shown in fig. 4: when welding, the temperature is too high or the time is too long, so that the electrical performance index in the crystal oscillator is abnormal, and the crystal oscillator does not start oscillation, therefore, the welding heat resistance of the crystal oscillator has important significance. In order to further test the influence of the silver alloy thin film on the stability of the crystal oscillator, the welding heat resistance of the load resonant Frequency (FL) and the Resonance Resistance (RR) after using different electrode films for different models of crystal oscillators was studied, and the result is shown in fig. 4 as the test result of the test environment of 265 ℃ ± 5 ℃ for the test time of 10s,1 cycle. It can be seen that the 7M26M crystal oscillator using the palladium-copper electrode film, after being subjected to the soldering heat resistance test, found that the amount of change in FL frequency was less than 1.15ppm, exhibiting good frequency heat resistance stability. Similarly, in the case of a 7M26M crystal oscillator using an Ag film as an electrode, the frequency heat resistance stability was poor, the amount of change was about 4.25ppm, and the stability was lower than that of the sample using the APC electrode film. Indicating that the frequency stability of the ACP electrode film is superior to that of the Ag film. The above results indicate that the welding heat resistance of the product using the palladium-copper thin film as the electrode is superior to that of the product using Ag as the electrode for the 7M26M crystal oscillator.
The vacuum coating process comprises the following steps:
s1, cleaning and preparing a coating chamber. Because the cover of the vacuum chamber is difficult to open, the cover can be easily taken down after the vacuum chamber is inflated for a period of time. Cleaning the film coating chamber, removing residual metal in the vacuum chamber, and cleaning the deposit on the wall with alcohol. The metal tin wires are folded into hook shapes, 6 tin wires are adopted and placed on the metal tungsten wires, and the metal tin wires can be preferably in full contact with the tungsten wires, but cannot enable the tungsten wires to be partially in short circuit.
S2, preparing a substrate: and (4) cleaning the glass slide. The substrate is mounted on the top of the vacuum chamber, and the vacuum chamber is closed.
And S3, turning on a power supply of the composite vacuum machine, and preheating for ten minutes.
And S4, switching on a power supply of the electronic diffractometer, pulling the three-way valve outwards to the bottom, starting the mechanical pump (at the moment, starting pumping the vacuum chamber by the mechanical pump), firstly driving the composite vacuum meter to a left measurement gear, observing the change of the pointer, finding that the change is slow, then driving to a right measurement gear, finding that the index change of the pointer is fast, and indicating that the measurement gear on the right side measures the air pressure of the vacuum chamber.
And S5, beating the composite vacuum meter to the right measuring gear, observing the readings, beating the composite vacuum meter to the left measuring gear when the readings are lower than 6.7 Pa, then pushing the three-way valve to the bottom, still making the readings lower than 6.7 Pa, beating the composite vacuum meter to the right measuring gear again, observing the readings (the pressure of the vacuum chamber at the moment), and if the readings are higher than 6.7 Pa, pulling the three-way valve to the bottom outwards, and continuously pumping the vacuum chamber by the mechanical pump. Similarly, if the gas pressure of the gas storage cylinder is higher than 6.7 Pa, the three-way valve still needs to be pushed inwards to the bottom after the vacuum chamber is pumped out, and the mechanical pump is used for pumping the gas storage chamber. The air pressure of the vacuum chamber and the air storage bottle is repeatedly pumped by a mechanical pump, and the air pressure of the air storage bottle in the vacuum chamber is required to be lower than 6.7 Pa.
And S6, switching on cooling water, turning on an oil diffusion pump, and preheating for 40 minutes.
S7, after preheating is finished, the pressure of the vacuum chamber and the pressure of the gas storage bottle are both lower than 6.7 Pa, the measuring gear is driven to the right side, the three-way valve is pushed inwards to the bottom, and then the high-vacuum butterfly valve is opened.
And S8, observing the readings of the vacuum gauge, turning on a lamp filament when the readings are lower than 0.1 Pa, turning on the ionization gauge, and continuously converting the maximum measuring range as required until the readings are less than 5 Pa (at the moment, turning off the ionization gauge, firstly turning off the lamp filament, and then turning off the ionization gauge).
S9, starting coating, shifting to a coating gear, then turning on a coating switch, gradually rotating the filament to adjust the coating, and increasing the current to 40A. And adjusting the current according to the heat red degree of the tungsten filament.
And S10, observing the film coating condition, and indicating that the film coating is finished when the red light of the tungsten filament is obviously shielded or the purple light similar to the side of a mirror appears from the side. Slowly turning off the current switch, and then turning off the coating switch and the coating baffle.
And S11, closing the high vacuum butterfly valve and cutting off the power supply of the oil diffusion pump.
And S12, after cooling for a plurality of minutes, closing the mechanical pump, inflating the vacuum chamber, opening the film coating chamber after the inflation is finished, taking out the sample, and observing the film coating condition.
And S13, cutting off the cooling water when the oil diffusion pump is cooled to the room temperature. And (5) arranging the instruments.
Attention points in vacuumizing:
an oil diffusion pump:
1. before starting, the vacuum degree of the vacuum chamber and the gas storage bottle must be pre-pumped to be more than 6.7 Pa, and cooling water is introduced before heating
2. When in use, the condition that whether the oil diffusion pump is in the working requirement is constantly concerned
3. After the experiment, the ionization vacuum gauge is turned off, the oil diffusion pump is turned off before inflation, the power supply of the heating furnace is turned off before shutdown, and the cooling water is turned off after cooling for 20 minutes
Ionization gauge:
1. before high vacuum measurements, attention was paid to the range of use of ionization gauges: a vacuum degree of 10-1 Pa or more (or a pressure of 10-1 Pa or less), so that the vacuum degree is higher than 10 -1 Handkerchief;
2. in the high vacuum measurement, the predicted use condition is not met with the possibility of the predicted experimental condition;
3. after high vacuum measurement, when the device is shut down, the ionization gauge is firstly closed, and then the high vacuum butterfly valve is closed;
cooling water:
1. before the oil diffusion pump is heated, cooling water is introduced at the same time;
2. when the oil diffusion pump is used, whether the water temperature and the flow are normal or not is noticed at all times;
3. after the oil diffusion pump is cooled to the room temperature, the mechanical pump is closed, and finally the cooling water is closed;
the annealing process comprises the following steps:
when annealing is carried out, the annealing temperature of the tubular furnace is set to be 800 ℃, the film is placed into the tubular furnace, and nitrogen is introduced at the same time. Then raising the temperature to 800 ℃ at the speed of 5-10 ℃ per minute, and preserving the temperature for 30 minutes; the temperature was then lowered to 600 ℃ and held for an additional 30 minutes. Thereafter, the temperature was then increased from 600 ℃ to 700 ℃ and held for another 30 minutes, after which the temperature was decreased to 500 ℃ and held for another 30 minutes. Next, the temperature was raised from 500 ℃ to 600 ℃ for another 30 minutes, after which the temperature was lowered to 400 ℃ for another 30 minutes. The temperature of each time can be up to 50 ℃ or down, wherein the temperature is 800 ℃,700 ℃, 600 ℃ and 500 ℃.
As shown in FIG. 5, where the left side is before baking and the right side is at a baking temperature of 325 deg.C, the grain size of the alloy is not substantially changed as the baking temperature in vacuum increases (325 deg.C). However, compared with the common annealing process, the annealing method adopting the multiple-advancing and multiple-retreating can inhibit the increase of the grain size to a certain extent and improve the thermal stability.
Claims (5)
1. An electrode of a silver palladium copper crystal oscillator is characterized in that: the specific components comprise silver, palladium and copper, and form an alloy material.
2. The silver palladium copper crystal oscillator electrode of claim 1, wherein: also includes indium, iron and selenium.
3. The silver palladium copper crystal oscillator electrode of claim 2, wherein: the specific contents are 97.65 percent to 98.124 percent of Ag, 0.86 percent to 1.25 percent of Pd, 0.62 percent to 0.94 percent of Cu, 0.42 percent to 0.69 percent of In, 0.20 percent to 0.35 percent of Te and 0.16 percent to 0.28 percent of Se according to the mass ratio.
4. The silver palladium copper crystal oscillator electrode coating process according to claim 1, 2 or 3, characterized by comprising the following steps:
the method comprises the following steps: cleaning a coating chamber;
step two: preparing a substrate, cleaning a glass slide, and closing a vacuum chamber;
step three: starting a power supply of the vacuum machine, and preheating for 8-15 minutes;
step four: switching on a power supply of the electron diffractometer;
step five: keeping the air pressure of the vacuum chamber and the air storage bottle of the vacuum chamber to be 5-6.7 Pa;
step six: cooling water is connected, an oil diffusion pump is started, and preheating is carried out for 30-50 minutes;
step seven: after preheating, observing the readings of the vacuum gauge, turning on a lamp filament when the readings are lower than 0.1 Pa, switching on an ionization gauge, and continuously converting the maximum measuring range until the readings are lower than 5 Pa;
step eight: the current is adjusted according to the hot red degree of the tungsten filament when the film coating is started;
step nine: observing the film coating condition, and when the red light of the tungsten filament is shielded, slowly closing the current switch after film coating is finished, and then closing the film coating switch and the film coating baffle;
step ten: closing the high vacuum butterfly valve and cutting off the power supply of the oil diffusion pump;
step eleven: cooling for 5-10 min, closing the mechanical pump, inflating the vacuum chamber, opening the coating chamber after inflation, taking out the product, and observing the coating condition;
step twelve: and (6) ending.
5. The silver palladium copper crystal oscillator electrode coating annealing process according to claim 1, 2 or 3, characterized by comprising the following steps:
the method comprises the following steps: putting into a coating, increasing the speed of 5-10 ℃ per minute to 700-900 ℃, and keeping for 25-35 minutes;
step two: cooling to 550-650 deg.C, and maintaining for 25-35 min;
step three: heating to 700-750 deg.c for 25-35 min;
step four: cooling to 450-550 deg.C, and maintaining for 25-35 min;
step five: heating to 600-650 deg.C, and maintaining for 25-35 min;
step six: cooling to 350-450 deg.c and maintaining for 25-35 min;
step seven: stopping heating and naturally cooling.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116247442A (en) * | 2023-02-06 | 2023-06-09 | 广东福顺天际通信有限公司 | Electromagnetic wave lens and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116247442A (en) * | 2023-02-06 | 2023-06-09 | 广东福顺天际通信有限公司 | Electromagnetic wave lens and production method thereof |
| CN116247442B (en) * | 2023-02-06 | 2024-02-23 | 广东福顺天际通信有限公司 | Electromagnetic wave lens and production method thereof |
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