CN110455793B - Method for distinguishing pure titanium and titanium alloy - Google Patents
Method for distinguishing pure titanium and titanium alloy Download PDFInfo
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- CN110455793B CN110455793B CN201910805740.5A CN201910805740A CN110455793B CN 110455793 B CN110455793 B CN 110455793B CN 201910805740 A CN201910805740 A CN 201910805740A CN 110455793 B CN110455793 B CN 110455793B
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The present disclosure provides a method for distinguishing pure titanium from titanium alloy, the method comprises the following specific steps: (1) firstly, polishing a sample; (2) respectively carrying out ultrasonic cleaning on the polished sample by using absolute ethyl alcohol and acetone, and then carrying out vacuum drying; (3) finally, one or more corrosive solutions in inorganic acid, organic matters or salt solutions are used for preparing corrosive solutions, the cleaned samples are placed into the corrosive solutions for reaction, and judgment is carried out according to the color of the reaction solutions after the reaction is finished; the standard of color judgment is as follows: if the reaction solution is blue, the sample is titanium alloy; the reaction solution is purple or purple red, and the sample is pure titanium. The method is simple to operate, can simply distinguish pure titanium and titanium alloy, does not need a precise instrument, can distinguish in a common laboratory, and has the advantages of simplicity, convenience and saving.
Description
Technical Field
The disclosure belongs to the technical field of titanium processing, and particularly relates to a method for distinguishing pure titanium and titanium alloy.
Background
Because titanium and titanium alloy have very good heat resistance, intensity, plasticity, toughness, formability, weldability, corrosion resistance and biocompatibility, so the materials used by implants such as dental implant, artificial joint, intraosseous fixation device and the like at present are mainly pure titanium and titanium alloy, wherein the most common pure titanium is TA4 pure titanium, the most common titanium alloy is TC4, and the composition of TC4 material is Ti-6 AL-4V. There is a risk of mixing titanium and titanium alloys during the actual production process, which may adversely affect the machining process or the subsequent surface treatment process. Because there is no significant difference in appearance, density and other properties between pure titanium and titanium alloy, it is reported that the method can distinguish industrial pure titanium and titanium alloy by sampling, calcining and observing the color of oxide film with naked eyes. The pure titanium and the titanium alloy can be distinguished by using instruments, and a spectrometer or an X-ray fluorescence spectrometer and a thermoelectric comparator are commonly used for distinguishing the pure titanium and the titanium alloy, but the instruments have the disadvantages of high purchase cost, large occupied space and large-size inconvenience in movement.
Disclosure of Invention
The purpose of the present disclosure is to provide a method for distinguishing pure titanium from titanium alloy, so as to achieve the purpose of simply distinguishing pure titanium from titanium alloy.
In order to realize the purpose, the technical scheme is as follows:
a method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively carrying out ultrasonic cleaning on the polished sample by using absolute ethyl alcohol and acetone, and then carrying out vacuum drying;
(3) finally, one or more corrosive solutions in inorganic acid, organic matters or salt solutions are used for preparing corrosive solutions, the cleaned samples are placed into the corrosive solutions for reaction, and judgment is carried out according to the color of the reaction solutions after the reaction is finished;
the standard of color judgment is as follows: if the reaction solution is blue, the sample is titanium alloy; the reaction solution is purple or purple red, and the sample is pure titanium.
The frequency of ultrasonic cleaning is 6-24KHz, the cleaning frequency is 2-3 times, and the ultrasonic cleaning time is 3-5 min.
The vacuum degree of the vacuum drying is 0.025-0.045MPa, and the vacuum drying time is 5-10 min.
The inorganic acid and alkali is sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide or potassium hydroxide.
The organic matter is hexane, diethyl ether, ethanol, methanol, ethylenediamine, formic acid or acetic acid.
The salt solution is ferric chloride solution, zinc chloride solution, magnesium chloride solution, calcium chloride solution, zinc chloride solution, barium chloride solution or nickel chloride solution.
The corrosive solution in the step (3) comprises 10-100% by mass of H2SO4The reaction temperature is 40-120 ℃, and the reaction time is 5-10min。
The corrosive solution in the step (3) comprises 10-40% by mass of H2SO4And 3-10% by volume of HF, H2SO4And the addition ratio of HF is (10-250): (0.1-1), the reaction temperature is room temperature, and the reaction time is 0.5-30 min.
The corrosive solution in the step (3) comprises 1-35% by mass of HCl and 5-40% by mass of H2SO4HCl and H2SO4The addition ratio of (1-250): (0.1-1), the reaction temperature is 25-45 ℃, and the reaction time is 2-20 min.
The corrosive solution in the step (3) comprises 1-20 mass percent of HNO3And 3-10% by mass of HF, HNO3And the addition ratio of HF is (1-2.5): (0.5-1), the reaction temperature is 25-45 ℃, and the reaction time is 2-20 min.
The corrosive solution in the step (3) comprises a magnesium chloride solution with the mass fraction of 40% -50% and a calcium chloride solution with the mass fraction of 55% -65%, and the adding proportion of the magnesium chloride solution to the calcium chloride solution is (1-3): (2-5), the reaction temperature is 120-160 ℃, and the reaction time is 25-50 min.
The corrosive solution in the step (3) comprises 100% by mass of HCl and absolute ethyl alcohol, wherein the addition ratio of the 100% by mass of HCl to the absolute ethyl alcohol is 2: 100, the reaction temperature is 25-35 ℃, and the reaction time is 30-45 min.
The beneficial effects of this disclosure are: the method has the advantages that the method is simple to operate, can simply distinguish the pure titanium and the titanium alloy, does not need a precise instrument, can distinguish the pure titanium and the titanium alloy in a common laboratory, and has the advantages of simplicity, convenience and saving.
Detailed Description
The following steps are only used for illustrating the technical scheme of the disclosure and are not limited; although the present disclosure has been described in detail with reference to the foregoing steps, those of ordinary skill in the art will understand that: the technical solutions recorded in the foregoing steps may still be modified, or some or all of the technical features may be equivalently replaced; and such modifications or substitutions do not depart from the scope of the respective technical solutions of the steps of the present disclosure.
Example 1
A method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively carrying out ultrasonic (24KHz) cleaning on the sample for 2 times with 5min each time by using absolute ethyl alcohol and acetone, and then carrying out vacuum drying for 10min under the vacuum degree of 0.025 MPa;
(3) mixing 40% of H2SO4And 3% by volume of HF, in an addition ratio of 10: 0.1, preparing a corrosive solution, then putting the dried sample into the corrosive solution for reaction, wherein the reaction temperature is room temperature, the reaction time is 30min, and after the reaction is finished, judging according to the color of the reaction solution;
the standard of color judgment is as follows: the reaction solution is blue, and the material is titanium alloy; the reaction solution is purple, purple red, light red or light purple, and the material is pure titanium.
Example 2
A method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively carrying out ultrasonic (6KHz) cleaning on the sample for 3 times by using absolute ethyl alcohol and acetone, wherein the cleaning time is 10min each time, and then carrying out vacuum drying for 5min under the vacuum degree of 0.045 MPa;
(3) mixing 35% of HCl and 5% of H by mass2SO4HCl and H2SO4The addition ratio of (1): 1 preparing corrosive solution, then putting the dried sample into the corrosive solution for reaction, wherein the reaction temperature is 45 ℃, and the reaction temperature isThe time is 2min, and after the reaction is finished, the judgment is carried out according to the color of the reaction solution;
the standard of color judgment is as follows: the reaction solution is blue, and the material is titanium alloy; the reaction solution is purple, purple red, light red or light purple, and the material is pure titanium.
Example 3
A method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively ultrasonically (15KHz) cleaning the sample for 3 times with anhydrous ethanol and acetone for 8min, and vacuum drying under vacuum degree of 0.035MPa for 8 min;
(3) adding a 42% magnesium chloride solution and a 65% calcium chloride solution according to the addition ratio of 1: 2, preparing a corrosive solution, then putting the dried sample into the corrosive solution for reaction, wherein the reaction temperature is 160 ℃, the reaction time is 50min, and after the reaction is finished, judging according to the color of the reaction solution;
the standard of color judgment is as follows: the reaction solution is blue, and the material is titanium alloy; the reaction solution is purple, purple red, light red or light purple, and the material is pure titanium.
Example 4
A method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively ultrasonically cleaning the sample for 2 times (18KHz) with anhydrous ethanol and acetone for 6min, and vacuum drying under vacuum degree of 0.04MPa for 6 min;
(3) adding HCl with the mass fraction of 100% and absolute ethyl alcohol according to the addition ratio of 2: 100, preparing a corrosive solution, then putting the dried sample into the corrosive solution for reaction, wherein the reaction temperature is 25 ℃, the reaction time is 30min, and after the reaction is finished, judging according to the color of the reaction solution;
the standard of color judgment is as follows: the reaction solution is blue, and the material is titanium alloy; the reaction solution is purple, purple red, light red or light purple, and the material is pure titanium.
Example 5
A method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively ultrasonically cleaning the sample for 2 times (18KHz) with anhydrous ethanol and acetone for 6min, and vacuum drying under vacuum degree of 0.03MPa for 9 min;
(3) HNO with the mass fraction of 20 percent3And 3% by mass of HF, HNO3And the addition ratio of HF is 2.5: 1, preparing a corrosive solution, then putting the dried sample into the corrosive solution for reaction, wherein the reaction temperature is 25 ℃, the reaction time is 20min, and after the reaction is finished, judging according to the color of the reaction solution;
the standard of color judgment is as follows: the reaction solution is blue, and the material is titanium alloy; the reaction solution is purple, purple red, light red or light purple, and the material is pure titanium.
Example 6
A method for distinguishing pure titanium from titanium alloy comprises the following specific steps:
(1) firstly, polishing a sample;
(2) respectively ultrasonically cleaning the sample for 3 times (18KHz) by using absolute ethyl alcohol and acetone, wherein the cleaning time is 6min each time, and then carrying out vacuum drying for 9min under the vacuum degree of 0.03 MPa;
(3) mixing 80% of H2SO4The sample is a corrosive solution, then the dried sample is put into the corrosive solution for reaction, wherein the reaction temperature is 45 ℃, the reaction time is 10min, and after the reaction is finished, the judgment is carried out according to the color of the reaction solution;
the standard of color judgment is as follows: the reaction solution is blue, and the material is titanium alloy; the reaction solution is purple, purple red, light red or light purple, and the material is pure titanium.
Claims (5)
1. A method for distinguishing pure titanium from titanium alloy is characterized by comprising the following specific steps:
(1) firstly, polishing a sample;
(2) respectively carrying out ultrasonic cleaning on the polished sample by using absolute ethyl alcohol and acetone, and then carrying out vacuum drying;
(3) finally, one or more corrosive solutions in inorganic acid, organic matters or salt solutions are used for preparing corrosive solutions, the samples after vacuum drying are placed into the corrosive solutions for reaction, and judgment is carried out according to the colors of the reaction solutions after the reaction is finished;
the standard of color judgment is as follows: if the reaction solution is blue, the sample is titanium alloy; if the reaction solution is purple or purple red, the sample is pure titanium;
in the step (3), the corrosive solution comprises 40% by mass of sulfuric acid and 3% by volume of hydrofluoric acid, and the addition ratio of the sulfuric acid to the hydrofluoric acid is 10: 0.1, the reaction temperature is room temperature, and the reaction time is 30 min;
or the corrosive solution comprises 35 mass percent of hydrochloric acid and 5 mass percent of sulfuric acid, and the adding proportion of the hydrochloric acid to the sulfuric acid is 1: 1, the reaction temperature is 45 ℃, and the reaction time is 2 min;
or the corrosive solution comprises 42 mass percent of magnesium chloride solution and 65 mass percent of calcium chloride solution, and the adding proportion of the magnesium chloride solution to the calcium chloride solution is 1: 2, the reaction temperature is 160 ℃, and the reaction time is 50 min;
or the corrosive solution comprises 100% by mass of hydrochloric acid and absolute ethyl alcohol, and the addition ratio of the hydrochloric acid to the absolute ethyl alcohol is 2: 100, the reaction temperature is 25 ℃, and the reaction time is 30 min;
or the corrosive solution comprises 20 mass percent of nitric acid and 3 volume percent of hydrofluoric acid, and the addition ratio of the nitric acid to the hydrofluoric acid is 2.5: 1, the reaction temperature is 25 ℃, and the reaction time is 20 min;
or the corrosive solution comprises 80 mass percent of sulfuric acid, the reaction temperature is 45 ℃, and the reaction time is 10 min.
2. The method of distinguishing between pure titanium and titanium alloys according to claim 1 wherein said ultrasonic cleaning is at a frequency of: 16-24 KHz.
3. The method for distinguishing pure titanium from titanium alloys according to claim 1, wherein the number of ultrasonic cleaning is 2-3 times and the ultrasonic cleaning time is 3-5 min.
4. The method of distinguishing between pure titanium and titanium alloys of claim 1 wherein said vacuum drying is performed at a vacuum level of 0.025 to 0.045 MPa.
5. The method of differentiating pure titanium from titanium alloys according to claim 1, wherein said vacuum drying time is 5-10 min.
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| CN110455793B true CN110455793B (en) | 2021-12-14 |
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Patent Citations (7)
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| EP1373875A2 (en) * | 2001-04-02 | 2004-01-02 | Zeptosens AG | Optical structure for multi-photon excitation and the use thereof |
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| CN104807811A (en) * | 2015-05-11 | 2015-07-29 | 梧州市产品质量检验所 | Method for detecting titanium dioxide in ore |
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Address after: 528000 unit 602, 6th floor, block a, Jingu Photoelectric Industrial community, No.1, Yongan North Road, Pingzhou, Guicheng Street, Nanhai District, Foshan City, Guangdong Province Patentee after: Guangdong Zhongke Anchi Biotechnology Co.,Ltd. Address before: 528000 unit 602, 6th floor, block a, Jingu Photoelectric Industrial community, No.1, Yongan North Road, Pingzhou, Guicheng Street, Nanhai District, Foshan City, Guangdong Province Patentee before: FOSHAN ANGELS BIOTECHNOLOGY Co.,Ltd. |