CN114351094A - Production method of micro-balance quartz wafer with plating-enhanced graphite layer - Google Patents
Production method of micro-balance quartz wafer with plating-enhanced graphite layer Download PDFInfo
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- CN114351094A CN114351094A CN202111566259.9A CN202111566259A CN114351094A CN 114351094 A CN114351094 A CN 114351094A CN 202111566259 A CN202111566259 A CN 202111566259A CN 114351094 A CN114351094 A CN 114351094A
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- quartz wafer
- graphite layer
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- microbalance quartz
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Abstract
The invention discloses a production method of a graphite layer plating-increasing microbalance quartz wafer, which comprises the following steps: plating a metal film on the microbalance quartz wafer to obtain a metal-plated microbalance quartz wafer; plating a graphite layer on the metal coating microbalance quartz wafer to obtain the microbalance quartz wafer with the plated graphite layer, wherein the sputtering power of a metal coating on the microbalance quartz wafer is 0.30kW-0.40kW, the vacuum degree of the graphite layer plating on the metal coating microbalance quartz wafer is 5.0 multiplied by 10 < -1 > Pa-7.0 multiplied by 10 < -1 > Pa, the pre-heating coating temperature before coating is 120 ℃ -140 ℃, the sputtering power is 0.5kW to 0.8kW, and the speed is 0.0 multiplied by 10 < -1 > Pa
Description
Technical Field
The invention relates to the field of precision instruments, in particular to a production method of a microbalance quartz wafer with a plating-increasing graphite layer.
Background
The quartz crystal microbalance is based on the acoustic wave sensing principle, adopts a modular design, and can detect the tiny mass and structure changes on the surface of a chip through the frequency change and the dissipation change of a quartz sensor. Suitable for both gas and liquid samples. The method has a frequency doubling operation mode, can give information such as viscosity, elastic modulus, viscous modulus, thickness and the like of the film, can be used for detecting gas phase components and toxic explosive gases, and has the advantages of good specificity, high sensitivity, low cost, simplicity and convenience in operation and the like. In order to increase the sensitivity of the metal film-coated microbalance quartz wafer to the object to be measured, a graphite layer is generally coated on the metal film. However, the smoothness of the metal film in the prior art is not enough, so that the adhesion degree of the graphite layer is poor, the graphite layer is wrinkled and falls off, and the adhesion degree of the graphite film sensitive film is poor due to the technology of plating the graphite layer in the prior art.
Disclosure of Invention
In order to solve the problem that the graphite layer of the microbalance quartz wafer with the plating-increasing graphite layer is wrinkled and falls off, the invention provides the following scheme:
a production method of a graphite layer-coated microbalance quartz wafer comprises the following steps:
plating a metal film on the microbalance quartz wafer to obtain a metal-plated microbalance quartz wafer;
plating a graphite layer on the metal-coated microbalance quartz wafer to obtain a graphite layer-plated microbalance quartz wafer,
the sputtering power for plating the metal film on the microbalance quartz wafer is 0.30kw-0.40kw,
the vacuum degree of the graphite layer added on the quartz wafer of the metal coating microbalance is 5.0 multiplied by 10 < -1 > Pa to 7.0 multiplied by 10 < -1 > Pa, the preheating coating temperature before coating is 120 ℃ to 140 ℃, the sputtering power is 0.5kW to 0.8kW, and the speed is
According to the embodiment of the invention, the vacuum degree of plating a metal film on the microbalance quartz wafer is 4.0 x 10 < -1 > Pa to 5.4 x 10 < -1 > Pa, the temperature of heating and plating the film before plating is 90 ℃ to 105 ℃, and the rate is
According to the embodiment of the invention, the final graphite thickness in the graphite layer-added microbalance quartz wafer obtained by adding the graphite layer to the metal-coated microbalance quartz wafer is 100 nm-150 nm.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The production method of the graphite layer-added microbalance quartz wafer comprises two steps:
step 1: plating a metal film on the microbalance quartz wafer to obtain the metal film-plated microbalance quartz wafer, wherein the process comprises the following steps: sputtering power of 0.30-0.40 kw, vacuum degree of 4.0 × 10-1Pa-5.4 × 10-1Pa, heating coating temperature of 90-105 deg.C before coating, and rate of
After the sputtering power is increased, the surface roughness of the metal film coated microbalance quartz wafer can be increased, but the premise is that the gold electrode film is ensured not to generate obvious gold particles, otherwise, the good measuring range and the precision of the microbalance are reduced.
Step 2: and plating a graphite layer on the metal coated microbalance quartz wafer to obtain the graphite layer plated microbalance quartz wafer, wherein the process comprises the following steps: the vacuum degree is 5.0 multiplied by 10 < -1 > Pa to 7.0 multiplied by 10 < -1 > Pa, the pre-heating coating temperature before coating is 120 ℃ to 140 ℃, and the sputtering power is0.5kW to 0.8kW at a rate of
The parameters are actually carried out on the premise of ensuring the good measuring range and precision of the microbalance. The final graphite layer thickness in the obtained metal coating-enhanced microbalance quartz wafer is 100 nm-150 nm by respectively improving the vacuum degree of the graphite layer enhanced coating of the metal coating-enhanced microbalance quartz wafer, the pre-heating coating temperature before coating, the sputtering power and the rate.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The process for obtaining the metal coating microbalance quartz wafer comprises the following steps: the sputtering power is 0.38kw, the vacuum degree is 4.8 multiplied by 10 < -1 > Pa, the heating coating temperature before coating is 99 ℃, and the speed is
The process for obtaining the plating-increased graphite layer microbalance quartz wafer comprises the following steps: the vacuum degree is 5.9 multiplied by 10 < -1 > Pa, the pre-heating coating temperature before coating is 128 ℃, the sputtering power is 0.6kW, and the speed is
And the thickness of the final graphite layer in the obtained plating-increasing graphite layer microbalance quartz wafer is 120 nm.
Example 2
The process for obtaining the metal coating microbalance quartz wafer comprises the following steps: the sputtering power is 0.39kw, the vacuum degree is 5.2X 10-1Pa, the heating coating temperature before coating is 102 ℃, and the rate is
The process for obtaining the plating-increased graphite layer microbalance quartz wafer comprises the following steps: the vacuum degree is 6.3 multiplied by 10 < -1 > Pa, the pre-heating coating temperature before coating is 134 ℃, the sputtering power is 0.7kW, and the speed is
Obtaining a final graphite layer in the plating-increasing graphite layer microbalance quartz waferThe thickness was 130 nm.
The graphite layer of the microbalance quartz wafer with the additional plating graphite layer has no failure phenomena such as wrinkling, falling and the like, and the sensitivity of the microbalance quartz wafer can be ensured.
Although the description herein refers to embodiments, it is not intended that each embodiment cover a separate embodiment, but rather that each embodiment cover a separate embodiment, and that such references are made for clarity only, as those skilled in the art will recognize: the technical solutions in the embodiments may be combined to form other embodiments as understood by those skilled in the art, taking the description as a whole.
Claims (3)
1. A production method of a graphite layer-coated microbalance quartz wafer comprises the following steps:
plating a metal film on the microbalance quartz wafer to obtain a metal-plated microbalance quartz wafer;
plating a graphite layer on the metal-coated microbalance quartz wafer to obtain a graphite layer-plated microbalance quartz wafer,
the sputtering power for plating the metal film on the microbalance quartz wafer is 0.30kw-0.40kw,
the vacuum degree of the graphite layer added on the quartz wafer of the metal coating microbalance is 5.0 multiplied by 10 < -1 > Pa to 7.0 multiplied by 10 < -1 > Pa, the preheating coating temperature before coating is 120 ℃ to 140 ℃, the sputtering power is 0.5kW to 0.8kW, and the speed is
2. The method for producing the graphite layer coated microbalance quartz wafer according to claim 1, wherein the degree of vacuum for coating the microbalance quartz wafer with the metal film is 4.0 x 10 "1 Pa to 5.4 x 10" 1Pa, the temperature of the heat coating before coating is 90 ℃ to 105 ℃ and the rate is
3. The method for producing the increased graphite layer coated microbalance quartz wafer according to claim 1, wherein the final graphite thickness of the increased graphite layer coated microbalance quartz wafer obtained by increasing graphite layer on the metal coated microbalance quartz wafer is 100nm to 150 nm.
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| CN202111566259.9A CN114351094B (en) | 2021-12-20 | 2021-12-20 | Production method of plating graphite layer microbalance quartz wafer |
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| CN202111566259.9A CN114351094B (en) | 2021-12-20 | 2021-12-20 | Production method of plating graphite layer microbalance quartz wafer |
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Citations (8)
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|---|---|---|---|---|
| US5428882A (en) * | 1993-04-05 | 1995-07-04 | The Regents Of The University Of California | Process for the fabrication of aluminum metallized pyrolytic graphite sputtering targets |
| US20040135467A1 (en) * | 2002-12-27 | 2004-07-15 | Nihon Dempa Kogyo Co., Ltd. | Method of manufacturing thin quartz crystal wafer |
| CN203299075U (en) * | 2013-07-04 | 2013-11-20 | 长沙理工大学 | Aluminum base quartz crystal microbalance sensor with three layers of metal films |
| CN203324133U (en) * | 2013-07-04 | 2013-12-04 | 长沙理工大学 | Quartz crystal microbalance sensor based on copper-based three-layer metal film |
| US20140361665A1 (en) * | 2013-06-10 | 2014-12-11 | Nihon Dempa Kogyo Co., Ltd. | Quartz crystal device and method for fabricating the same |
| WO2017107307A1 (en) * | 2015-12-22 | 2017-06-29 | 成都泰美克晶体技术有限公司 | Quartz crystal resonator having circular wafer structure and method for manufacturing same |
| CN106939405A (en) * | 2017-03-23 | 2017-07-11 | 南京信息工程大学 | A kind of preparation method of graphene/oxide complex optical film |
| WO2019042549A1 (en) * | 2017-08-30 | 2019-03-07 | Institut Za Fiziku | Process for forming ready-to-use qcm sensors with atomically flat surface suitable for stm measurements |
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2021
- 2021-12-20 CN CN202111566259.9A patent/CN114351094B/en active Active
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|---|---|---|---|---|
| US5428882A (en) * | 1993-04-05 | 1995-07-04 | The Regents Of The University Of California | Process for the fabrication of aluminum metallized pyrolytic graphite sputtering targets |
| US20040135467A1 (en) * | 2002-12-27 | 2004-07-15 | Nihon Dempa Kogyo Co., Ltd. | Method of manufacturing thin quartz crystal wafer |
| US20140361665A1 (en) * | 2013-06-10 | 2014-12-11 | Nihon Dempa Kogyo Co., Ltd. | Quartz crystal device and method for fabricating the same |
| CN203299075U (en) * | 2013-07-04 | 2013-11-20 | 长沙理工大学 | Aluminum base quartz crystal microbalance sensor with three layers of metal films |
| CN203324133U (en) * | 2013-07-04 | 2013-12-04 | 长沙理工大学 | Quartz crystal microbalance sensor based on copper-based three-layer metal film |
| WO2017107307A1 (en) * | 2015-12-22 | 2017-06-29 | 成都泰美克晶体技术有限公司 | Quartz crystal resonator having circular wafer structure and method for manufacturing same |
| CN106939405A (en) * | 2017-03-23 | 2017-07-11 | 南京信息工程大学 | A kind of preparation method of graphene/oxide complex optical film |
| WO2019042549A1 (en) * | 2017-08-30 | 2019-03-07 | Institut Za Fiziku | Process for forming ready-to-use qcm sensors with atomically flat surface suitable for stm measurements |
Non-Patent Citations (1)
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| 赵双琦;刘桂礼;李东;刘刚;: "石英晶片镀膜频率监控技术研究", 真空科学与技术学报, no. 05 * |
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