CN111472041A - Piezoelectric type force sensor XY crystal group processing method - Google Patents

Piezoelectric type force sensor XY crystal group processing method Download PDF

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Publication number
CN111472041A
CN111472041A CN201910991474.XA CN201910991474A CN111472041A CN 111472041 A CN111472041 A CN 111472041A CN 201910991474 A CN201910991474 A CN 201910991474A CN 111472041 A CN111472041 A CN 111472041A
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crystal
growth
seed
seed crystal
temperature
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金雷
孟亚静
孙佳宝
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Liaoning Provincial College of Communications
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Liaoning Provincial College of Communications
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/18Quartz
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/16Measuring force or stress, in general using properties of piezoelectric devices

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A piezoelectric type force sensor XY crystal group processing method comprises the following steps: s1: controlling the temperature by using a constant-temperature power temperature controller, selecting high-quality natural quartz, secondary smelting and tertiary smelting quartz crystals for the culture body respectively, and selecting high-quality artificial crystals for the seed crystals; s2: corroding the seed crystal by adopting an ammonia hydrofluoride solution; s3, fixing seed crystals at two ends of a conductive metal sheet which does not react with the growth liquid, blocking the seed crystal wafer in the Z direction by the metal sheet, placing the seed crystal wafer in a growth area in a high-pressure kettle in a crystal growth environment, fixing the seed crystal wafer and the metal sheet together, hanging the seed crystal wafer and the metal sheet on a seed crystal frame, and growing the quartz crystal in a unidirectional mode along the Z direction without the blocking of a copper sheet; s4; fixing the quartz crystal and external restraint, hanging the quartz crystal on a seed crystal frame, and placing the seed crystal frame in a factory for growth; s5: and when the crystal growth period is finished, cutting off a power supply, naturally cooling to 70 ℃, and opening the high-pressure kettle to take out the crystal. The invention can obtain a large amount of crystal groups in a short time, has better consistency, does not have a processing process in the thickness direction of the crystal groups and improves the mechanical property.

Description

Piezoelectric type force sensor XY crystal group processing method
Technical Field
The invention relates to a crystal group processing method, in particular to a piezoelectric type force sensor XY crystal group processing method.
Background
A piezoelectric force sensor is a device that measures a force, a load, and a moment acting on a piezoelectric crystal (generally quartz) based on a piezoelectric effect. The piezoelectric force sensor is mainly composed of a crystal group, the crystal group is formed by assembling double X or Y-shaped cutting wafers, and normal load detection is carried out by using the XY crystal group.
The X-cut crystal group consists of two wafers and an electrode, and the traditional processing and assembling processes comprise processing the wafers and the electrode, cleaning and drying the wafers, then grinding, cleaning and drying the electrode, finally compressing the electrode wafers, and simultaneously performing waterproof treatment to form the crystal group. This method has certain disadvantages, the first is that the manual assembly has errors; secondly, the micro-damage in the wafer processing process affects the mechanical property of the wafer, and finally affects the reliability of the sensor.
The temperature of the artificial quartz is controlled by a constant temperature power temperature controller, the culture body respectively selects high-quality natural quartz, secondary smelting and tertiary smelting quartz crystals, the seed crystal selects high-quality artificial crystal, the seed crystal is corroded by the conventional hydrofluoric acid and is changed into ammonium hydrofluoride solution, a cosolvent is high-purity NaOH with the concentration of 1.2-1.5 mol/L, the temperature of a growth area is controlled to be 330-340 ℃, the temperature difference between a dissolving area and the growth area can be 30-50 ℃ according to the position difference of a temperature measuring point, the growth rate of the crystal is controlled to be 0.4-0.6 mm/d, the constant temperature time can be maintained to be 35-55 d according to the size requirement, the temperature rising process conforms to a certain program, when the growth period of the crystal is finished, a power supply is cut off, the natural temperature reduction temperature is reduced to 70 ℃, the kettle is opened, the crystal is taken out, the inner surface of an autoclave, a seed crystal frame and a material basket are thoroughly cleaned and coated, and the seed crystal and the raw materials are also strictly treated according to the set process.
In the traditional process, one side of a seed wafer in the Z direction is blocked by an iron sheet, the seed wafer and the iron sheet are fixed together through a steel wire and hung on a seed wafer frame, quartz grows unidirectionally along the Z direction, the iron sheet has the function of preventing bidirectional growth, as shown in figure 2, crystals can only grow in the direction shown by an arrow, and the obtained wafer is XY-cut. The traditional crystal growth process finally obtains a metal sheet and a Z-direction wafer with a certain thickness, and the other side wafer is still lacked between the obtained structure and the crystal group.
Disclosure of Invention
In order to solve the technical problems, the invention provides a new processing method aiming at an XY crystal group required by normal load detection, and the technical scheme is as follows:
a piezoelectric type force sensor XY crystal group processing method is characterized by comprising the following steps:
s1: controlling the temperature by using a constant-temperature power temperature controller, selecting high-quality natural quartz, secondary smelting and tertiary smelting quartz crystals for the culture body respectively, and selecting high-quality artificial crystals for the seed crystals;
s2: corroding the seed crystal by adopting an ammonia hydrofluoride solution;
s3, fixing seed crystals at two ends of a conductive metal sheet which does not react with the growth liquid, blocking the seed crystal wafer in the Z direction by the metal sheet, placing the seed crystal wafer in a growth area in a high-pressure kettle in a crystal growth environment, fixing the seed crystal wafer and the metal sheet together, hanging the seed crystal wafer and the metal sheet on a seed crystal frame, and growing the quartz crystal in a unidirectional mode along the Z direction without the blocking of a copper sheet;
s4; fixing the quartz crystal and external restraint, hanging the quartz crystal on a seed crystal frame, and placing the seed crystal frame in a factory for growth;
s5: and when the crystal growth period is finished, cutting off a power supply, naturally cooling to 70 ℃, and opening the high-pressure kettle to take out the crystal.
And the cosolvent adopted in the corrosion process in the step S2 is high-purity NaOH with the concentration of 1.2-1.5 mol/L.
In the step S3, the temperature of the growth area is controlled to be 330-340 ℃, and the temperature difference between the dissolution area and the growth area can be 30-50 ℃ according to the position of the temperature measuring point.
The growth rate of the crystal is controlled to be 0.4-0.6 mm/d, and the growth rate is constant under a specific temperature and pressure, so the constant temperature time is maintained to be 35-55 d.
In step S4, a through hole is formed in the side of the external restraint body.
In step S4, the external restraint body is made of a metal material that is resistant to high temperature and does not react with the growth liquid.
The wafer thickness is controlled by the growth time, which can be controlled by applying external constraints. When the growth time is controlled, the growth speed of the crystal in the high-temperature axe is calculated, and the growth time is accurately controlled.
Compared with the prior art, the invention has the beneficial effects that:
1. a large amount of crystal groups can be obtained in a short time, and 200-300 crystal groups can be obtained in one crystal growth process;
2. the consistency of the crystal group is better, and a multidirectional load sensor is further packaged;
3. no processing process is carried out in the thickness direction of the crystal group, and the mechanical property index of the crystal group is expected to be greatly improved;
4. the mechanical property is improved, and a small-size wide-range sensor becomes possible.
Drawings
FIG. 1 is a schematic diagram of the crystal structure;
FIG. 2 is a schematic view showing the fixing condition of seed crystal and the direction of crystal growth;
FIG. 3 is a schematic diagram of a crystal group obtained by using a crystal growth process;
FIG. 4 is a schematic view of growth in a constrained state.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the 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.
Example 1
As shown in fig. 3, the seed crystal is fixed at both ends of the copper sheet (in the Z direction), the copper sheet is placed in a crystal growth environment, the crystal grows along both ends of the copper electrode, and with the growth completion, a crystal group consisting of XY cut wafers is finally obtained.
Example 2
The problem of uneven upper and lower surfaces of a crystal group can be solved by an external constraint forming mode, a quartz crystal is placed in an external constraint body, the external constraint body is similar to a sensor shell, as shown in figure 4, a large number of through holes are formed in the side part of the external constraint body, gasified quartz saturated solution can freely enter and exit, a copper electrode and upper and lower seed crystals are fixed in the copper electrode, the quartz crystal grows in the external constraint body, when the quartz crystal grows to a certain thickness, a gap between the crystal and the external constraint body is small, the gasified quartz saturated solution is prevented from further contacting with the crystal in the thickness direction, and the crystal stops growing. The external constraint forming mode also optimizes the growth time, prevents the continuous growth of the crystal from causing internal fragmentation, and reduces the probability of deformity caused by the growth of the crystal along the XY direction.
Example 3
In order to keep the purity of the growth system, the inner surface of the autoclave, the seed crystal frame and the charging basket need to be thoroughly cleaned and coated, and the seed crystal and the raw materials are strictly treated according to the set process.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (6)

1. A piezoelectric type force sensor XY crystal group processing method is characterized by comprising the following steps:
s1: controlling the temperature by using a constant-temperature power temperature controller, selecting high-quality natural quartz, secondary smelting and tertiary smelting quartz crystals for the culture body respectively, and selecting high-quality artificial crystals for the seed crystals;
s2: corroding the seed crystal by adopting an ammonia hydrofluoride solution;
s3, fixing seed crystals at two ends of a conductive metal sheet which does not react with the growth liquid, blocking the seed crystal wafer in the Z direction by the metal sheet, placing the seed crystal wafer in a growth area in a high-pressure kettle in a crystal growth environment, fixing the seed crystal wafer and the metal sheet together, hanging the seed crystal wafer and the metal sheet on a seed crystal frame, and growing the quartz crystal in a unidirectional mode along the Z direction without the blocking of a copper sheet;
s4; fixing the quartz crystal and external restraint, hanging the quartz crystal on a seed crystal frame, and placing the seed crystal frame in a factory for growth;
s5: and when the crystal growth period is finished, cutting off a power supply, naturally cooling to 70 ℃, and opening the high-pressure kettle to take out the crystal.
2. The method as claimed in claim 1, wherein the co-solvent used in the etching process in step S2 is high purity NaOH with a concentration of 1.2-1.5 mol/L.
3. The method for processing the XY crystal group of the piezoelectric force sensor according to claim 1, wherein the temperature of the growth region is controlled to be 330-340 ℃ in step S3, and the temperature difference between the dissolution region and the growth region is 30-50 ℃ according to the position of the temperature measurement point.
4. The method as claimed in claim 1, wherein the crystal growth rate is controlled to be 0.4-0.6 mm/d, and the growth rate is controlled to be constant at a specific temperature and pressure, so that the crystal growth rate is controlled by controlling the time, and the constant temperature time is maintained to be 35-55 d.
5. The method as claimed in claim 1, wherein the external constraining member has through holes at its side in step S4.
6. The method as claimed in claim 1, wherein the external constraining body is made of a metal material resistant to high temperature and non-reactive with the growth liquid in step S4.
CN201910991474.XA 2019-10-18 2019-10-18 Piezoelectric type force sensor XY crystal group processing method Pending CN111472041A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112899778A (en) * 2021-01-21 2021-06-04 烁光特晶科技有限公司 Method for manufacturing deep ultraviolet high-transmittance quartz crystal

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000264786A (en) * 1999-03-16 2000-09-26 Nippon Dempa Kogyo Co Ltd Production of synthetic quartz, synthetic quartz produced with the same and quartz wafer from the same synthetic quartz
JP2000272999A (en) * 1999-03-24 2000-10-03 Nippon Dempa Kogyo Co Ltd Method for controlling etched channel generated in artificial quartz and method for processing artificial quartz and high grade artificial quartz, quartz wafer and quartz piece by the methods

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000264786A (en) * 1999-03-16 2000-09-26 Nippon Dempa Kogyo Co Ltd Production of synthetic quartz, synthetic quartz produced with the same and quartz wafer from the same synthetic quartz
JP2000272999A (en) * 1999-03-24 2000-10-03 Nippon Dempa Kogyo Co Ltd Method for controlling etched channel generated in artificial quartz and method for processing artificial quartz and high grade artificial quartz, quartz wafer and quartz piece by the methods

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
樊尚春等: "《信号与测试技术》", 30 April 2011, 北京航空航天大学出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112899778A (en) * 2021-01-21 2021-06-04 烁光特晶科技有限公司 Method for manufacturing deep ultraviolet high-transmittance quartz crystal
CN112899778B (en) * 2021-01-21 2022-02-01 烁光特晶科技有限公司 Method for manufacturing deep ultraviolet high-transmittance quartz crystal

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Application publication date: 20200731