CN114112606A - Preparation method of titanium alloy bolt head crystal grain streamline sample - Google Patents

Preparation method of titanium alloy bolt head crystal grain streamline sample Download PDF

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Publication number
CN114112606A
CN114112606A CN202111318063.8A CN202111318063A CN114112606A CN 114112606 A CN114112606 A CN 114112606A CN 202111318063 A CN202111318063 A CN 202111318063A CN 114112606 A CN114112606 A CN 114112606A
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China
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titanium alloy
bolt head
sample
alloy bolt
crystal grain
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CN202111318063.8A
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Inventor
贾智宇
邬建新
赵兴丽
张媛媛
王娜
陈程
李慧
王景海
张敬彤
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Shaanxi Aircraft Industry Co Ltd
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Shaanxi Aircraft Industry Co Ltd
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Priority to CN202111318063.8A priority Critical patent/CN114112606A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Sampling And Sample Adjustment (AREA)

Abstract

The application provides a preparation method of a TC4 titanium alloy bolt head crystal grain streamline sample, and belongs to the technical field of aviation. The method comprises the following steps: embedding and grinding a titanium alloy bolt head crystal grain streamline sample; processing a titanium alloy bolt head crystal grain streamline sample by using a prepared corrosive agent, and drying the sample by blowing, wherein the corrosive agent comprises at least three of hydrofluoric acid analytical reagent, hydrochloric acid analytical reagent, nitric acid analytical reagent, sulfuric acid analytical reagent, acetic acid analytical reagent, alcohol, copper sulfate and deionized water; and determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope, and finally, intuitively and clearly displaying the TC4 titanium alloy bolt head crystal grain streamline.

Description

Preparation method of titanium alloy bolt head crystal grain streamline sample
Technical Field
The application belongs to the technical field of aviation, and particularly relates to a preparation method of a titanium alloy bolt head crystal grain streamline sample.
Background
The defects of the existing bolt forging piece not only cause the performance of the bolt to be poor, but also even seriously restrict the service life of the finished product. Therefore, the bolt forging is subjected to head crystal grain streamline inspection, and has important significance in actual production.
For the TC4 titanium alloy bolt, whether the grain streamline at the upset can be clearly shown or not and the complete grain streamline distribution information is obtained becomes the key of whether the accurate and reliable evaluation result can be finally obtained or not.
Disclosure of Invention
In order to solve the problem that the complete grain streamline distribution information of the grain streamline at the TC4 titanium alloy bolt head cannot be clearly shown in the prior art, the application provides a sample preparation method capable of visually and clearly displaying the grain streamline at the TC4 titanium alloy bolt head, and the technical scheme is as follows:
a method for preparing a sample of a TC4 titanium alloy bolt head grain streamline. The method comprises the following steps:
embedding and grinding a titanium alloy bolt head crystal grain streamline sample;
processing a titanium alloy bolt head crystal grain streamline sample by using a prepared corrosive agent, and drying the sample by blowing, wherein the corrosive agent comprises at least three of hydrofluoric acid analytical reagent, hydrochloric acid analytical reagent, nitric acid analytical reagent, sulfuric acid analytical reagent, acetic acid analytical reagent, alcohol, copper sulfate and deionized water;
and determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope.
Optionally, the prepared corrosive agent consists of 5ml to 10ml of hydrofluoric acid analytically pure, 10ml to 30ml of nitric acid analytically pure and 30ml to 60ml of deionized water.
Optionally, the prepared etchant consists of 5ml of hydrofluoric acid analytically pure, 15ml of nitric acid analytically pure, and 30ml of deionized water.
Optionally, the prepared etchant consists of 8ml of hydrofluoric acid analytically pure, 15ml of nitric acid analytically pure, and 37ml of deionized water.
Optionally, the prepared etchant consists of 10ml of hydrofluoric acid analytically pure, 30ml of nitric acid analytically pure, and 60ml of deionized water.
Optionally, the insert milled titanium alloy bolt head grain flow line sample comprises:
and (3) roughly grinding the embedded titanium alloy bolt head crystal grain streamline sample, wherein 180# waterproof abrasive paper is adopted for rough grinding, and then 400# waterproof abrasive paper, 800# waterproof abrasive paper and 1200# waterproof abrasive paper are adopted for fine grinding in sequence.
Optionally, the step of performing corrosion treatment on the flow line sample of the crystal grains at the head of the titanium alloy bolt after insert grinding by using the prepared corrosive agent, and drying the sample by blowing includes:
putting the prepared titanium alloy bolt head crystal grain streamline sample into a beaker with corrosive agent,
taking out a titanium alloy bolt head crystal grain streamline sample from the beaker after a preset time;
washing the taken out titanium alloy bolt head crystal grain streamline sample and wiping the sample with alcohol;
and drying the wiped titanium alloy bolt head crystal grain streamline sample.
Optionally, the preset time is 1-3 minutes.
The preparation method of the titanium alloy bolt head crystal grain streamline sample can clearly display the TC4 titanium alloy bolt head crystal grain streamline.
Drawings
FIG. 1 is a flow chart of a method for preparing a titanium alloy bolt head grain flow line sample provided herein;
FIG. 2 is a flow chart of a method for preparing a titanium alloy bolt head grain streamline sample provided by the present application.
Detailed Description
The present application will now be described in further detail with reference to the following detailed description of illustrative embodiments thereof, which are illustrated in the accompanying drawings.
The application provides a preparation method of a titanium alloy bolt head crystal grain streamline sample, wherein the titanium alloy bolt head crystal grain streamline sample is the titanium alloy bolt head crystal grain streamline sample, and as shown in figure 1, the method comprises the following steps:
step 110, embedding and grinding a titanium alloy bolt head crystal grain streamline sample.
And 120, carrying out corrosion treatment on the crystal grain streamline sample at the head part of the titanium alloy bolt after the embedded grinding by adopting the prepared corrosive, and drying.
The corrosive agent comprises at least three of hydrochloric acid analytically pure, nitric acid analytically pure, sulfuric acid analytically pure, acetic acid analytically pure, alcohol, copper sulfate and deionized water.
And step 130, determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope.
And (4) determining the metallographic structure of the titanium alloy bolt head grain streamline sample by adopting a metallographic microscope, namely completing the preparation of the titanium alloy bolt head grain streamline sample.
The application provides a preparation method of a titanium alloy bolt head crystalline grain streamline sample, which is used for the titanium alloy bolt head crystalline grain streamline sample, the prepared corrosive is adopted to carry out corrosion treatment on the titanium alloy bolt head crystalline grain streamline sample after being embedded and ground, and the titanium alloy bolt head crystalline grain streamline sample is dried. The method is simple and easy to implement, has little harm to the environment and the body of a tester, and can control the test time.
Optionally, the corrosive agent consists of 5ml to 10ml of hydrofluoric acid analytically pure, 10ml to 30ml of nitric acid analytically pure and 30ml to 60ml of deionized water, so that the proportion of the hydrofluoric acid is reduced, the volatilization of acid liquor is reduced, the harm to a human body is greatly reduced, and the environment is protected; during coarse grinding and fine grinding, the test sample is ground by the same method, and the test sample needs to be cleaned when the sand paper is replaced once, and the test sample is rotated by 45-90 degrees by taking the normal direction of a grinding surface as a rotation center, so that the grinding mark of the sand paper in the previous time is removed; the specific corrosion process is that the prepared sample is put into a beaker with corrosive liquid and taken out after being corroded for a certain time; and determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope.
Alternatively, the etchant may be comprised of 5ml to 10ml of hydrofluoric acid analytically pure, 10ml to 30ml of nitric acid analytically pure, 30ml to 60ml of deionized water.
The application also provides a preparation method of the titanium alloy bolt head crystal grain streamline sample, and the titanium alloy bolt head crystal grain streamline sample is the titanium alloy bolt head crystal grain streamline sample. As shown in fig. 2, the method includes:
step 210, preparing a corrosive agent.
The etchant consisted of 5ml of hydrofluoric acid analytically pure, 15ml of nitric acid analytically pure, and 30ml of deionized water.
And step 220, carrying out coarse grinding and fine grinding on the inlaid titanium alloy bolt head crystal grain streamline sample.
The coarse grinding is carried out by using 180# waterproof abrasive paper, and then fine grinding is carried out by sequentially using 400# waterproof abrasive paper, 800# waterproof abrasive paper and 1200# waterproof abrasive paper.
And 230, putting the prepared titanium alloy bolt head crystal grain streamline sample into a beaker with corrosive agent.
And step 240, taking out the titanium alloy bolt head crystal grain streamline sample from the beaker after a preset time.
The preset time is 1-3 minutes.
And step 250, flushing the taken out titanium alloy bolt head grain streamline sample and wiping the sample by using alcohol.
And step 260, drying the wiped titanium alloy bolt head crystal grain streamline sample.
And 270, determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope.
The application provides a preparation method of a titanium alloy bolt head crystalline grain streamline sample, which is used for the titanium alloy bolt head crystalline grain streamline sample, the prepared corrosive agent is adopted to corrode the titanium alloy bolt head crystalline grain streamline sample after being embedded and ground, and the titanium alloy bolt head crystalline grain streamline sample is dried. The method is simple and easy to implement, has little harm to the environment and the body of a tester, and can control the test time.
The application also provides a preparation method of the titanium alloy bolt head crystal grain streamline sample, and the titanium alloy bolt head crystal grain streamline sample is the titanium alloy bolt head crystal grain streamline sample. The method comprises the following steps:
and 310, preparing a corrosive agent, wherein the corrosive agent consists of 8ml of hydrofluoric acid analytically pure, 15ml of nitric acid analytically pure and 37ml of deionized water.
And step 320, carrying out coarse grinding and fine grinding on the embedded titanium alloy bolt head grain streamline sample, wherein 180# waterproof abrasive paper is adopted for the coarse grinding, and then 400# waterproof abrasive paper, 800# waterproof abrasive paper and 1200# waterproof abrasive paper are adopted for fine grinding in sequence.
Step 330, placing the prepared titanium alloy bolt head grain streamline sample into a beaker with corrosive agent.
And 340, taking out the titanium alloy bolt head crystal grain streamline sample from the beaker after a preset time.
The preset time is 1-3 minutes.
And 350, washing the taken out titanium alloy bolt head crystal grain streamline sample and wiping the sample with alcohol.
And 360, drying the wiped titanium alloy bolt head crystal grain streamline sample.
And 370, determining the metallographic structure of the processed titanium alloy bolt head grain streamline sample by adopting a metallographic microscope.
The application provides a preparation method of a titanium alloy bolt head crystalline grain streamline sample, which is used for the titanium alloy bolt head crystalline grain streamline sample, the prepared corrosive agent is adopted to corrode the titanium alloy bolt head crystalline grain streamline sample after being embedded and ground, and the titanium alloy bolt head crystalline grain streamline sample is dried. The method is simple and easy to implement, has little harm to the environment and the body of a tester, and can control the test time.
The application also provides a preparation method of the titanium alloy bolt head crystal grain streamline sample, and the titanium alloy bolt head crystal grain streamline sample is the titanium alloy bolt head crystal grain streamline sample. The method comprises the following steps:
step 410, preparing a corrosive agent, wherein the corrosive agent consists of 10ml of hydrofluoric acid analytically pure, 30ml of nitric acid analytically pure and 60ml of deionized water.
And step 420, carrying out coarse grinding and fine grinding on the embedded titanium alloy bolt head grain streamline sample, wherein 180# waterproof abrasive paper is adopted for the coarse grinding, and then 400# waterproof abrasive paper, 800# waterproof abrasive paper and 1200# waterproof abrasive paper are adopted for fine grinding in sequence.
Step 430, putting the prepared titanium alloy bolt head grain streamline sample into a beaker with corrosive agent.
And 440, taking out the titanium alloy bolt head crystal grain streamline sample from the beaker after a preset time.
The preset time is 1-3 minutes.
And 450, washing the taken out titanium alloy bolt head grain streamline sample and wiping the sample with alcohol.
Step 460, drying the wiped titanium alloy bolt head grain streamline sample.
And 470, determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope.
In addition, in this embodiment, the etchant may consist of 92ml of analytically pure hydrochloric acid, 5ml of analytically pure sulfuric acid and 3ml of analytically pure nitric acid, or 1.5g of copper sulfate, 40ml of analytically pure hydrochloric acid and 20ml of alcohol, or 50ml of analytically pure hydrochloric acid, 5ml of analytically pure nitric acid and 50ml of deionized water.
The foregoing merely represents embodiments of the present application, which are described in greater detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application.

Claims (8)

1. A preparation method of a titanium alloy bolt head crystal grain streamline sample is characterized by comprising the following steps:
embedding and grinding a titanium alloy bolt head crystal grain streamline sample;
processing a titanium alloy bolt head crystal grain streamline sample by using a prepared corrosive agent, and drying the sample by blowing, wherein the corrosive agent comprises at least three of hydrofluoric acid analytical reagent, hydrochloric acid analytical reagent, nitric acid analytical reagent, sulfuric acid analytical reagent, acetic acid analytical reagent, alcohol, copper sulfate and deionized water;
and determining the metallographic structure of the processed titanium alloy bolt head crystal grain streamline sample by adopting a metallographic microscope.
2. The method of claim 1,
the prepared corrosive agent consists of 5ml to 10ml of hydrofluoric acid analytically pure, 10ml to 30ml of nitric acid analytically pure and 30ml to 60ml of deionized water.
3. The method of claim 2,
the prepared corrosive agent consists of 5ml of hydrofluoric acid analytically pure, 15ml of nitric acid analytically pure and 30ml of deionized water.
4. The method of claim 2,
the prepared corrosive agent consists of 8ml of hydrofluoric acid analytically pure, 15ml of nitric acid analytically pure and 37ml of deionized water.
5. The method of claim 2,
the prepared corrosive agent consists of 10ml of hydrofluoric acid analytically pure, 30ml of nitric acid analytically pure and 60ml of deionized water.
6. The method of claim 1,
the inlay and grind titanium alloy bolt head crystalline grain streamline sample includes:
and (3) roughly grinding the embedded titanium alloy bolt head crystal grain streamline sample, wherein 180# waterproof abrasive paper is adopted for rough grinding, and then 400# waterproof abrasive paper, 800# waterproof abrasive paper and 1200# waterproof abrasive paper are adopted for fine grinding in sequence.
7. The method of claim 1,
adopt the good corrosive agent of preparation to carry out corrosion treatment to the titanium alloy bolt head crystalline grain streamline sample after inlaying the mill to weather, include:
putting the prepared titanium alloy bolt head crystal grain streamline sample into a beaker with corrosive agent, and taking out the titanium alloy bolt head crystal grain streamline sample from the beaker after a preset time;
washing the taken out titanium alloy bolt head crystal grain streamline sample and wiping the sample with alcohol; and drying the wiped titanium alloy bolt head crystal grain streamline sample.
8. The method of claim 7,
the preset time is 1-3 minutes.
CN202111318063.8A 2021-11-08 2021-11-08 Preparation method of titanium alloy bolt head crystal grain streamline sample Pending CN114112606A (en)

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CN112538629A (en) * 2020-11-16 2021-03-23 飞而康快速制造科技有限责任公司 Metallographic corrosive liquid and metallographic corrosive method for additive manufacturing of high-temperature alloy
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