CN110455793A - Method for distinguishing pure titanium and titanium alloy - Google Patents
Method for distinguishing pure titanium and titanium alloy Download PDFInfo
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- CN110455793A CN110455793A CN201910805740.5A CN201910805740A CN110455793A CN 110455793 A CN110455793 A CN 110455793A CN 201910805740 A CN201910805740 A CN 201910805740A CN 110455793 A CN110455793 A CN 110455793A
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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
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- 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
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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 titanium processing technique field, and in particular to a method of distinguish pure titanium and titanium alloy.
Background technique
Due to titanium and titanium alloy have good heat resistance, intensity, plasticity, toughness, formability, solderability, corrosion resistance and
Biocompatibility, so the material that the implantation materials such as dental implant, joint prosthesis, bone inner fixing device use at present is mainly pure titanium
With titanium alloy, the pure titanium of most common of them is the pure titanium of TA4, and most common titanium alloy is TC4, and wherein the group of TC4 material becomes Ti-
6AL-4V.There are the risks of titanium and titanium alloy mixing in actual production process, at process for machining or subsequent surface
Science and engineering skill brings unfavorable influence.Because there was no significant difference in the performances such as appearance, density for pure titanium and titanium alloy, it has been reported that
After sampling, calcining can be used, oxidation film color is detected by an unaided eye to distinguish technical pure titanium or titanium alloy, in this way speed
And unhappy and again relatively elaborate, poor reliability.Instrument can also be used to distinguish to pure titanium and titanium alloy, the most commonly used is make
Identify the difference of titanium and titanium alloy with spectrometer or x-ray fluorescence spectrometry instrument and thermoelectric comparator, but these instruments have
There are buying expenses high, occupy biggish space, and instrument is relatively large is inconvenient to move.
Summary of the invention
Purpose of this disclosure is to provide a kind of methods for distinguishing pure titanium and titanium alloy, simply distinguish pure titanium and titanium conjunction to reach
The purpose of gold.
To achieve the above object, technical solution is as follows:
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) with dehydrated alcohol and acetone, to polishing, treated that sample is cleaned by ultrasonic respectively, is then dried in vacuo；
(3) corrosive solution finally prepared using one or more of inorganic acid, organic matter or salting liquid, will clean
Sample afterwards, which is put into corrosive solution, to react, and after the reaction was completed, is judged according to the color of reaction solution；
The wherein standard of color judgement are as follows: reaction solution is blue, then sample is titanium alloy；Reaction solution is purple or purple
Red, then sample is pure titanium.
The frequency 6-24KHz of the ultrasonic cleaning, the number of cleaning are 2-3 times, and the ultrasonic cleaning time is 3-5min.
The vacuum drying vacuum degree is 0.025-0.045MPa, and the vacuum drying time is 5-10min.
The inorganic acid alkali is sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide or potassium hydroxide.
The organic matter is hexane, ether, ethyl alcohol, methanol, ethylenediamine, formic acid or acetic acid.
The salting liquid is ferric chloride solution, liquor zinci chloridi, magnesium chloride solution, calcium chloride solution, liquor zinci chloridi, chlorine
Change barium solution or nickel chloride solution.
Corrosive solution group is divided into the H of mass fraction 10%-100% in the step (3)2SO4, the reaction temperature is
40-120 DEG C, reaction time 5-10min.
The group of corrosive solution is divided into the H of mass fraction 10%-40% in the step (3)2SO4With volume fraction 3%-
10% HF, H2SO4Adding proportion with HF is (10-250): (0.1-1), reaction temperature are room temperature, reaction time 0.5-
30min。
The group of corrosive solution is divided into the HCl and mass fraction 5%- of mass fraction 1%-35% in the step (3)
40% H2SO4, HCl and H2SO4Adding proportion be (1-250): (0.1-1), the temperature of reaction is 25-45 DEG C, the reaction time
For 2-20min.
The group of corrosive solution is divided into the HNO of mass fraction 1%-20% in the step (3)3With mass fraction 3%-
10% HF, HNO3Adding proportion with HF is (1-2.5): (0.5-1), and reaction temperature is 25-45 DEG C, reaction time 2-
20min。
The group of corrosive solution is divided into the magnesium chloride solution and matter of mass fraction 40%-50% in the step (3)
The adding proportion of amount score 55%-65% calcium chloride solution, magnesium chloride solution and calcium chloride solution is (1-3): (2-5), reaction
Temperature is 120-160 DEG C, reaction time 25-50min.
The group of corrosive solution is divided into mass fraction 100%HCl and dehydrated alcohol in the step (3), wherein matter
It measures score 100%HCl and dehydrated alcohol adding proportion is 2:100, reaction temperature is 25-35 DEG C, reaction time 30-45min.
The beneficial effect of the disclosure is: providing a kind of method for distinguishing pure titanium and titanium alloy, uses and beat in the method
Mill and ultrasonic cleaning handle the oxidation product and greasy dirt that can remove sample surfaces, and to reduce response error, vacuum drying can be prevented
Titanium and titanium alloy surface form oxidation film, in order to avoid influencing difference as a result, the method is easy to operate, can easily distinguish pure
Titanium and titanium alloy, do not need precision instrument, can distinguish in common laboratory, have the advantages that easy, saving.
Specific embodiment
Following steps are only to illustrate the technical solution of the disclosure, rather than its limitations；Although referring to These steps
The disclosure is described in detail, but those skilled in the art should understand that: it still can be to aforementioned each step
Technical solution documented by rapid is modified, or equivalent substitution of some or all of the technical features；And these
It modifies or replaces, the range of each step technique scheme of the disclosure that it does not separate the essence of the corresponding technical solution.
Embodiment 1
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) it carries out ultrasonic (24KHz) to sample with dehydrated alcohol and acetone respectively to clean 2 times, the time cleaned every time is
Then 5min carries out vacuum drying 10min in the case where vacuum degree is 0.025MPa；
(3) by the H of quality point 40%2SO4It is that 10:0.1 prepares corrosivity according to adding proportion with the HF of volume fraction 3%
Then sample after drying is put into corrosive solution and is reacted by solution, wherein reaction temperature is room temperature, and the reaction time is
30min is judged according to the color of reaction solution after the reaction was completed；
The wherein standard of color judgement are as follows: reaction solution is blue, then material is titanium alloy；Reaction solution is purple, purple
Red, light red or lilac, then material is pure titanium.
Embodiment 2
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) it carries out ultrasonic (6KHz) to sample with dehydrated alcohol and acetone respectively to clean 3 times, the time cleaned every time is
Then 10min carries out vacuum drying 5min in the case where vacuum degree is 0.045MPa；
(3) by the H of 35% HCl and mass fraction 5%2SO4, HCl and H2SO4Adding proportion be 1:1 prepare corrosivity
Then sample after drying is put into corrosive solution and is reacted by solution, wherein the temperature reacted is 45 DEG C, the reaction time is
2min is judged according to the color of reaction solution after the reaction was completed；
The wherein standard of color judgement are as follows: reaction solution is blue, then material is titanium alloy；Reaction solution is purple, purple
Red, light red or lilac, then material is pure titanium.
Embodiment 3
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) it carries out ultrasonic (15KHz) to sample with dehydrated alcohol and acetone respectively to clean 3 times, the time cleaned every time is
Then 8min carries out vacuum drying 8min in the case where vacuum degree is 0.035MPa；
It (3) is that 1:2 prepares corruption according to adding proportion by 65% calcium chloride solution of 42% magnesium chloride solution and mass fraction
Then sample after drying is put into corrosive solution and is reacted by corrosion solution, wherein reaction temperature is 160 DEG C, when reaction
Between judged according to the color of reaction solution after the reaction was completed for 50min；
The wherein standard of color judgement are as follows: reaction solution is blue, then material is titanium alloy；Reaction solution is purple, purple
Red, light red or lilac, then material is pure titanium.
Embodiment 4
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) it carries out ultrasonic (18KHz) to sample with dehydrated alcohol and acetone respectively to clean 2 times, the time cleaned every time is
Then 6min carries out vacuum drying 6min in the case where vacuum degree is 0.04MPa；
It (3) is that 2:100 prepares corrosive solution according to adding proportion, so by mass fraction 100%HCl and dehydrated alcohol
The sample after drying is put into corrosive solution afterwards and is reacted, wherein reaction temperature is 25 DEG C, reaction time 30min, instead
After the completion of answering, judged according to the color of reaction solution；
The wherein standard of color judgement are as follows: reaction solution is blue, then material is titanium alloy；Reaction solution is purple, purple
Red, light red or lilac, then material is pure titanium.
Embodiment 5
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) it carries out ultrasonic (18KHz) to sample with dehydrated alcohol and acetone respectively to clean 2 times, the time cleaned every time is
Then 6min carries out vacuum drying 9min in the case where vacuum degree is 0.03MPa；
(3) by the HNO of mass fraction 20%3With the HF of mass fraction 3%, HNO3Adding proportion with HF is 2.5:1, is matched
Then sample after drying is put into corrosive solution and is reacted by corrosive solution processed, wherein reaction temperature is 25 DEG C, reaction
Time is 20min, after the reaction was completed, is judged according to the color of reaction solution；
The wherein standard of color judgement are as follows: reaction solution is blue, then material is titanium alloy；Reaction solution is purple, purple
Red, light red or lilac, then material is pure titanium.
Embodiment 6
A method of distinguishing pure titanium and titanium alloy, the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) it carries out ultrasonic (18KHz) to sample with dehydrated alcohol and acetone respectively to clean 3 times, the time cleaned every time is
Then 6min carries out vacuum drying 9min in the case where vacuum degree is 0.03MPa；
(3) by the H of mass fraction 80%2SO4For corrosive solution, it is molten that the sample after drying is then put into corrosivity
Reacted in liquid, wherein reaction temperature be 45 DEG C, reaction time 10min, after the reaction was completed, according to the color of reaction solution come into
Row judgement；
The wherein standard of color judgement are as follows: reaction solution is blue, then material is titanium alloy；Reaction solution is purple, purple
Red, light red or lilac, then material is pure titanium.
Claims (8)
1. a kind of method for distinguishing pure titanium and titanium alloy, which is characterized in that the specific steps of the method are as follows:
(1) sample is subjected to grinding process first；
(2) with dehydrated alcohol and acetone, to polishing, treated that sample is cleaned by ultrasonic respectively, is then dried in vacuo；
(3) corrosive solution finally prepared using one or more of inorganic acid, organic matter or salting liquid, will be dried in vacuo
Sample afterwards, which is put into corrosive solution, to react, and after the reaction was completed, is judged according to the color of reaction solution；
The wherein standard of color judgement are as follows: reaction solution is blue, then sample is titanium alloy；Reaction solution is purple or purplish red
Color, then sample is pure titanium.
2. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that the ultrasonic cleaning
Frequency are as follows: 16-24KHz.
3. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that the ultrasonic cleaning
Number be 2-3 time, the ultrasonic cleaning time be 3-5min.
4. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that described vacuum drying
Vacuum degree is 0.025-0.045MPa.
5. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that described vacuum drying
Time is 5-10min.
6. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that the inorganic acid is sulphur
Acid, hydrochloric acid, hydrofluoric acid and nitric acid.
7. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that the organic matter is for oneself
Alkane, ether, ethyl alcohol, methanol, ethylenediamine, formic acid or acetic acid.
8. the method for differentiation pure titanium and titanium alloy according to claims 1, which is characterized in that the salting liquid is chlorine
Change ferrous solution, liquor zinci chloridi, magnesium chloride solution, calcium chloride solution, liquor zinci chloridi, barium chloride solution or nickel chloride solution.
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| CN201910805740.5A CN110455793B (en) | 2019-08-29 | 2019-08-29 | Method for distinguishing pure titanium and titanium alloy |
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| CN201910805740.5A CN110455793B (en) | 2019-08-29 | 2019-08-29 | Method for distinguishing pure titanium and titanium alloy |
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| CN108776149A (en) * | 2018-04-11 | 2018-11-09 | 清华大学 | A method of titanium and titanium alloy ingot casting super large crystal grain is characterized by anode oxidation method |
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2019
- 2019-08-29 CN CN201910805740.5A patent/CN110455793B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1373875A2 (en) * | 2001-04-02 | 2004-01-02 | Zeptosens AG | Optical structure for multi-photon excitation and the use thereof |
| CN1743508A (en) * | 2005-09-21 | 2006-03-08 | 中国海洋大学 | Chemical etching solution for titanium and titanium alloy |
| CN101393127A (en) * | 2008-10-21 | 2009-03-25 | 宝鸡市华西金属科技有限责任公司 | Method for rapidly identifying industrial pure titanium by spectrometer |
| CN104745822A (en) * | 2015-03-12 | 2015-07-01 | 南昌航空大学 | Method for extracting titanium ions from titanium alloy chemical-milling waste liquid |
| 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 |
| CN105572123A (en) * | 2015-12-28 | 2016-05-11 | 西北工业大学 | Method for determining mechanical properties of heated titanium alloy component based on oxidative color standard blocks |
| CN108776149A (en) * | 2018-04-11 | 2018-11-09 | 清华大学 | A method of titanium and titanium alloy ingot casting super large crystal grain is characterized by anode oxidation method |
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| Title |
|---|
| 李旭等: "工业纯钛的高温热氧化行为", 《中国有色金属学报》 * |
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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. |