CN114351094B - Production method of plating graphite layer microbalance quartz wafer - Google Patents
Production method of plating graphite layer microbalance quartz wafer Download PDFInfo
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- CN114351094B CN114351094B CN202111566259.9A CN202111566259A CN114351094B CN 114351094 B CN114351094 B CN 114351094B CN 202111566259 A CN202111566259 A CN 202111566259A CN 114351094 B CN114351094 B CN 114351094B
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Abstract
The invention discloses a production method of a plating graphite layer microbalance quartz wafer, which comprises the following steps: plating metal films on the microbalance quartz wafer to obtain a metal-plated microbalance quartz wafer; the plating graphite layer is added to the metal plating film micro balance quartz wafer to obtain a micro balance quartz wafer with a plating graphite layer, the sputtering power of the metal plating film of the micro balance quartz wafer is 0.30kW-0.40kW, the vacuum degree of the plating graphite layer of the metal plating film micro balance quartz wafer is 5.0x10 < -1 > Pa-7.0x10 < -1 > Pa, the preheating plating film temperature before plating is 120 ℃ to 140 ℃, the sputtering power is 0.5kW-0.8kW, and the speed is
Description
Technical Field
The invention relates to the field of precision instruments, in particular to a production method of a micro balance quartz wafer with a plating graphite layer.
Background
The quartz crystal microbalance is based on the acoustic wave sensing principle, adopts a modularized design, and can detect tiny mass and structural change of the chip surface through frequency change and dissipation change of a quartz sensor. Is suitable for gas and liquid samples. The method has a frequency multiplication 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 gas, 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 a metal film plated microbalance quartz wafer to the object under test, a graphite layer is typically added to the metal film. However, the smoothness of the metal film in the prior art is insufficient, so that the adhesion degree of the graphite layer is poor, wrinkling and falling of the graphite layer can be caused, 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 of wrinkling and falling of a graphite layer of a quartz wafer of a plating graphite layer microbalance, the invention provides the following scheme:
a method for producing a plating graphite layer microbalance quartz wafer comprises the following steps:
plating metal films on the microbalance quartz wafer to obtain a metal-plated microbalance quartz wafer;
plating the graphite layer on the metal plating film micro balance quartz wafer to obtain the plating graphite layer micro balance quartz wafer,
the sputtering power of the plating metal film of the microbalance quartz wafer is 0.30kw-0.40kw,
the vacuum degree of the plating graphite layer of the metal plating micro balance quartz wafer is 5.0x10 < -1 > Pa-7.0x10 < -1 > Pa, the preheating plating temperature before plating is 120 ℃ to 140 ℃, the sputtering power is 0.5kW-0.8kW, and the speed is the following
According to the embodiment of the invention, the vacuum degree of the metal plating film of the microbalance quartz wafer is 4.0x10 < -1 > Pa-5.4x10 < -1 > Pa, the heating and plating temperature before plating is 90 ℃ to 105 ℃ and the speed is
According to the embodiment of the invention, the final graphite thickness of the plating-added graphite layer micro balance quartz wafer obtained by plating the graphite layer on the metal plating micro balance quartz wafer is 100-150 nm.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The production method of the plating graphite layer microbalance quartz wafer comprises the following two steps:
step 1: plating metal film on the quartz crystal wafer of the microbalance to obtain the quartz crystal wafer of the metal plating film, which comprises the following steps: the sputtering power is 0.30kw-0.40kw, the vacuum degree is 4.0X10-1 Pa-5.4X10-1 Pa, the heating and coating temperature before coating is 90 ℃ to 105 ℃ and the speed is the sameAfter the sputtering power is improved, the surface roughness of the metal film plated micro balance quartz wafer can be improved, but the premise is that the gold electrode film is ensured not to generate obvious gold particles, otherwise, the good measuring range and the accuracy of the micro balance are reduced.
Step 2: adding a graphite layer to the metal-coated microbalance quartz wafer to obtain a graphite layer-added microbalance quartz wafer, wherein the process comprises the following steps: vacuum degree is 5.0X10-1 Pa-7.0X10-1 Pa, pre-heating coating temperature is 120-140 ℃, sputtering power is 0.5kW-0.8kW, and rate isThe parameters are performed on the premise of ensuring the good measuring range and accuracy of the microbalance. The final graphite layer thickness in the metal plating film micro balance quartz wafer is 100 nm-150 nm by respectively improving the vacuum degree of the plating graphite layer, the preheating plating temperature, the sputtering power and the sputtering rate of the metal plating film micro balance quartz wafer.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
The process for obtaining the metal-coated microbalance quartz wafer comprises the following steps: the sputtering power is 0.38kw, the vacuum degree is 4.8X10-1 Pa, the heating and coating temperature before plating is 99 ℃ and the speed is
The process for obtaining the plating graphite layer microbalance quartz wafer comprises the following steps: vacuum degree is 5.9X10-1 Pa, preheating coating temperature before coating is 128 ℃, sputtering power is 0.6kW, and speed isThe final graphite layer thickness in the obtained plating-increasing graphite layer microbalance quartz wafer is 120nm.
Example 2
The process for obtaining the metal-coated microbalance quartz wafer comprises the following steps: the sputtering power is 0.39kw, the vacuum degree is 5.2X10-1 Pa, the heating and coating temperature before plating is 102 ℃ and the speed is
The process for obtaining the plating graphite layer microbalance quartz wafer comprises the following steps: vacuum degree of 6.3X10-1 Pa, preheating coating temperature of 134 deg.C, sputtering power of 0.7kW, and rate ofThe final graphite layer thickness in the obtained plating-increasing graphite layer microbalance quartz wafer is 130nm.
The graphite layer of the quartz wafer of the microbalance with the plating graphite layer has no failure phenomena such as wrinkling, falling off and the like, and the sensitivity of the quartz wafer of the microbalance can be ensured.
While the present description describes embodiments in terms of individual embodiments, not every embodiment is meant to be a single embodiment, and such description is for clarity only, as will be appreciated by those skilled in the art: the technical solutions in the embodiments may be combined to form other embodiments that can be understood by those skilled in the art.
Claims (2)
1. A method for producing a plating graphite layer microbalance quartz wafer comprises the following steps:
plating metal films on the microbalance quartz wafer to obtain a metal-plated microbalance quartz wafer;
plating a graphite layer on the metal plating film micro balance quartz wafer to obtain the plating graphite layer micro balance quartz wafer, which is characterized in that,
the sputtering power of the plating metal film of the microbalance quartz wafer is 0.30kw-0.40kw, and the vacuum degree is 4.0x10 -1 Pa-5.4×10 -1 Pa, heating and coating temperature before plating is 90-105 ℃ and speed is
The vacuum degree of the plating graphite layer of the metal plating film micro balance quartz wafer is 5.0 multiplied by 10 -1 Pa-7.0×10 -1 Pa, preheating coating temperature of 120-140 ℃, sputtering power of 0.5-0.8 kW, and speed of rate of
2. The method for producing a plating-added graphite layer microbalance quartz wafer according to claim 1, wherein the final graphite thickness in the plating-added graphite layer microbalance quartz wafer obtained by plating the metal-plated graphite layer quartz wafer is 100nm to 150nm.
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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 |
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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 |
Family Cites Families (2)
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JP4334864B2 (en) * | 2002-12-27 | 2009-09-30 | 日本電波工業株式会社 | Thin plate crystal wafer and method for manufacturing crystal resonator |
JP6163023B2 (en) * | 2013-06-10 | 2017-07-12 | 日本電波工業株式会社 | Quartz device and method of manufacturing quartz device |
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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 |
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 |
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