CN113019953B - High-speed full-automatic spectral analysis and classification system and method for rare earth metal - Google Patents
High-speed full-automatic spectral analysis and classification system and method for rare earth metal Download PDFInfo
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Abstract
The invention relates to a rare earth metal high-speed full-automatic spectral analysis and classification system and method, the rare earth element content in the sample is greater than 50%, the system includes central control server, sample grip movement device, sample conveyer to be measured, analyzing the surface locating device, analyzing the surface processing unit, rare earth spectrum analyzer, automatic weighing apparatus, automatic marking apparatus and finished product classification apparatus; the sample clamping movement device adopts a high-precision numerical control system to accurately control the clamped sample to be detected to move in the horizontal X-axis direction, the Y-axis direction and the vertical Z-axis direction. The invention integrates sample processing, spectral analysis, sample weighing and automatic marking and classification, omits wet analysis processes of chip preparation sampling, dissolution and the like, has high analysis speed, high accuracy and strong instantaneity, completes all actions within 3 minutes, and meets the technical requirement of necessary inspection of the rare earth metal sample blocks.
Description
Technical Field
The invention belongs to the technical field of metal spectral analysis, and particularly relates to a high-speed full-automatic spectral analysis and classification system and an analysis method for rare earth metals (containing rare earth alloys, the same below) with the content of rare earth elements in a sample being more than 50%.
Background
Rare earth elements are known as industrial vitamins, have irreplaceable excellent magnetic, optical and electrical properties, and play a great role in improving product performance, increasing product varieties and improving production efficiency. Because of large action and small dosage of rare earth, the rare earth has become an important element for improving the product structure, improving the technological content and promoting the technical progress of the industry, and is widely applied to the fields of metallurgy, military, petrochemical industry, glass ceramics, agriculture, new materials and the like. The middle east has petroleum and China has rare earth, and the rare earth resource is a dominant and strategic mineral resource in China. The rare earth metals and alloys are mainly applied to the metallurgy and mechanical manufacturing industries at first, and for many years, the rare earth metal industry in China continuously improves the preparation technology and the product quality by virtue of the advantages of abundant rare earth resources and lower production cost, and particularly, the rare earth metal industry develops rapidly and the yield increases rapidly along with the increase of the requirements of the product application market in recent years.
Because of the similarity of the rare earth elements, the analysis of the rare earth elements is always a difficult technical problem, on one hand, although the ICP spectrometer can accurately realize the analysis of impurity elements in the rare earth elements, the analysis speed and the result accuracy of the high-content rare earth main mass distribution cannot match the requirements of the rare earth metal smelting process on quality control. On the other hand, because the rare earth metal value is high, the components of each sample need to be detected in the production process, the detection workload is large, and a rapid automatic means is urgently needed to solve the problem.
The problem of rapid analysis in a rare earth metal laboratory can be solved by adopting a spark direct-reading atomic emission spectrometry, but the processes of sampling, manual sample preparation, spectral analysis and the like are also needed, the time consumption is long, the representativeness is poor, and the requirement that an alloy sample block must be inspected cannot be met.
Disclosure of Invention
In view of the above technical problems, an object of the present invention is to provide a high-speed full-automatic spectrum analysis and classification system for rare earth metals, which integrates sample processing, spectrum analysis, classification, sample weighing and automatic marking; and wet analysis processes such as chip making, sampling, dissolving and the like are omitted, and the technical requirement of necessary inspection of the alloy sample blocks is met.
The invention also aims to provide a high-speed full-automatic spectrum analysis method for rare earth metal, which has the advantages of high analysis speed, high accuracy and strong instantaneity, and all actions are completed within 3 minutes.
In order to achieve the purpose, the invention provides the following technical scheme:
a rare earth metal high-speed full-automatic spectrum analysis and classification system, the rare earth element content in the sample is greater than 50%, the system includes central control server 1, sample grip movement device 2, sample conveyer 4 to be measured, analyzing the surface locating device 5, analyzing the surface processing unit 6, rare earth spectrum analyzer 7, automatic weighing apparatus 8, automatic marking apparatus 9 and finished product classification apparatus;
the sample clamping and moving device 2 adopts a high-precision numerical control system to accurately control the clamped sample to be detected to move in the horizontal X-axis direction, the Y-axis direction and the vertical Z-axis direction; the sample conveying device 4 to be tested, the analysis surface positioning device 5, the analysis surface processing device 6, the rare earth spectrum analyzer 7, the automatic weighing device 8, the automatic marking device 9 and the finished product grading and classifying device are sequentially arranged in parallel along the X-axis direction of the sample clamping and moving device 2;
the sample conveying device 4 to be tested is used for conveying a sample to be tested to the sampling point 3 of the sample clamping and moving device 2;
the analysis surface positioning device 5 is used for determining the position of an analysis surface on a sample to be detected;
the analysis surface processing device 6 is used for processing a groove on the analysis surface position of the sample to be detected, which is determined by the analysis surface positioning device 5, and processing a flat analysis surface in the groove, wherein the shape of the groove is matched with the shape of a boss on an analysis table of the rare earth spectrum analyzer 7, so that the analysis surface is in a closed argon atmosphere after the sample to be detected is installed on the analysis table of the rare earth spectrum analyzer 7;
the rare earth spectrum analyzer 7 realizes automatic electrode brushing, automatic regular internal standard calibration, automatic curve height standard calibration, classification of samples to be detected according to set component content classification rules, and storage of sample analysis results in a database of the central control server 1;
the automatic weighing device 8 is used for weighing the measured sample and transmitting the weight of the sample to the database of the central control server 1 for storage;
the automatic marking device 9 is used for marking a sample number at the specified position of the measured sample and storing the sample number into a database of the central control server 1;
the finished product grading and classifying device comprises a finished product conveyor belt, a classifying push rod 11 and a plurality of finished product classifying bins 10; be equipped with the finished product platform on the finished product conveyer belt, categorised push rod 11 sets up on the finished product platform, can push the sample into corresponding finished product classification storehouse 10 according to central control server 1's instruction.
The analysis surface positioning device 5 comprises two fixing plates which are vertical to each other, and a Y-direction positioning plate 12 and two Z-direction positioning plates which can move samples along the Y-axis direction and the Z-axis direction are respectively arranged on the two fixing plates, each positioning plate is provided with a corresponding sensor, the positioning plates are supported by a plurality of guide pillars, and each guide pillar is sleeved with a return spring; the two Z-direction positioning plates are a sample analysis surface edge Z-direction positioning plate 14 and a sample analysis surface center Z-direction positioning plate 17 which are arranged in parallel with each other and are matched with the sensor to judge whether the sample is a waste sample.
The analysis surface positioning device 5 further includes: a shell of the analysis surface positioning device provided with the two fixing plates, a Y-direction guide post 20, a Y-direction sensor 21, a sample analysis surface center Z-direction positioning post 13, a Z-direction edge guide post 16, a sample analysis surface center Z-direction sensor 18, a Z-direction center guide post 19 and a sample analysis surface edge Z-direction sensor 15; wherein:
a pair of horizontally arranged Y-direction guiding columns 20 are slidably mounted on the analysis surface positioning device shell along the Y-axis direction, the positive Y-axis end of the Y-direction guiding column 20 positioned in the analysis surface positioning device shell is provided with a nut, and the Y-direction positioning plate 12 is vertically and fixedly connected with the negative Y-axis end of the Y-direction guiding column 20 positioned outside the analysis surface positioning device shell; a return spring is arranged on the Y-direction guide column 20 between the Y-direction positioning plate 12 and the shell of the analysis surface positioning device; the Y-direction sensor 21 is arranged between the Y-direction positioning plate 12 and the analysis surface positioning device shell and is used for detecting whether the Y-direction positioning plate 12 moves to a limited position;
a pair of vertically arranged Z-direction edge guide posts 16 and a pair of vertically arranged Z-direction central guide posts 19 are slidably mounted on the analysis surface positioning device housing along the Z-axis direction, the Z-direction edge guide posts 16 and the Z-direction central guide posts 19 are mounted with nuts at the Z-axis negative ends inside the analysis surface positioning device housing, and the sample analysis surface edge Z-direction positioning plate 14 is horizontally and fixedly connected to the Z-axis positive ends of the Z-direction edge guide posts 16 outside the analysis surface positioning device housing; a return spring is arranged on a Z-direction edge guide post 16 between the Z-direction positioning plate 14 at the edge of the sample analysis surface and the shell of the analysis surface positioning device;
the sample analysis surface center Z-direction positioning plate 17 is horizontally and fixedly connected to the Z-axis positive end of the Z-direction center guide pillar 19 positioned outside the shell of the analysis surface positioning device, and the sample analysis surface center Z-direction positioning plate 17 is positioned below the sample analysis surface edge Z-direction positioning plate 14; the center Z-direction positioning column 13 of the sample analysis surface is vertically and fixedly connected to the middle part of the center Z-direction positioning plate 17 of the sample analysis surface, and the top end of the center Z-direction positioning column 13 of the sample analysis surface can upwards freely slide through a through hole in the middle part of the edge Z-direction positioning plate 14 of the sample analysis surface and protrude out of the surface of the edge Z-direction positioning plate 14 of the sample analysis surface; a return spring is arranged on a Z-direction central guide pillar 19 between the sample analysis surface central Z-direction positioning plate 17 and the analysis surface positioning device shell; the sample analysis surface edge Z-direction sensor 15 is positioned below the sample analysis surface edge Z-direction positioning plate 14, and the sample analysis surface center Z-direction sensor 18 is positioned below the sample analysis surface center Z-direction positioning plate 17 and is higher than the sample analysis surface edge Z-direction sensor 15.
The analysis surface processing device 6 is used for driving a milling cutter to rotate by a motor to process a sample analysis surface.
The metal protective covers are arranged on the periphery and the upper portion of the analysis surface processing device 6 to prevent metal scraps from splashing in the processing process, and one end of each metal protective cover is provided with an opening to facilitate the sample clamping movement device 2 to clamp a sample to be detected to enter and exit.
The sample marking method of the automatic marking device 9 comprises physical stamping, laser marking, pneumatic marking and surface printing.
The total flow analysis time for each sample was less than 3 minutes.
The rare earth metal is single rare earth metal, mixed rare earth metal or rare earth alloy with the content of rare earth elements being more than 50%.
A high-speed full-automatic spectral analysis and classification method for rare earth metals according to the system comprises the following steps:
s1, sample conveying and clamping:
after cooling down the rare earth metal sample to be tested which is cast into a fixed pattern by a sampling mould, placing the rare earth metal sample to be tested on a sample to be tested conveying device 4, moving the sample to be tested to a sampling point 3 by the sample to be tested conveying device 4, and controlling a sample clamping moving device 2 to clamp the sample to be tested by a central control server 1;
s2, analyzing the position determination and judging the waste sample:
the sample clamping and moving device 2 moves the sample to be detected to the analysis surface positioning device 5 so as to determine the analysis surface position of the sample to be detected and judge whether the sample is a waste sample;
s3, analyzing surface processing:
the sample clamping and moving device 2 moves a sample to be tested to the analysis surface processing device 6, a groove is processed on the analysis surface position determined by the analysis surface positioning device 5, a flat analysis surface is processed in the groove, the shape of the groove is matched with the shape of a boss on an analysis table of the rare earth spectrum analyzer 7, and the air tightness in the analysis process is ensured;
s4, spectral analysis;
s5, classification:
the rare earth spectrum analyzer 7 classifies according to the shape and size of the sample and the analysis results of the rare earth elements, the alloy elements and the impurity elements to be detected, and transmits the analysis result data, the classification level and the sample number to the database of the central control server 1;
s6, weighing:
the sample clamping and moving device 2 moves the sample from the analysis table of the rare earth spectrum analyzer 7 to the automatic weighing device 8, puts down the sample, weighs, transmits the weight data to the database of the central control server 1, and matches the corresponding serial number; grabbing a sample for the second time;
s7, moving the sample to the automatic marking device 9 by the sample clamping and moving device 2, and printing a sample number at the designated position on the surface of the sample;
and S8, the sample clamping and moving device 2 moves the sample to a finished product table of the finished product conveyor belt, and the classification push rod 11 ejects the sample from the conveyor belt to the finished product classification bin 10 according to the classification result.
In said step S1, the sample temperature is <40 ℃.
In step S2, the sample clamping and moving device 2 clamps the sample to be measured and presses the Y-directional positioning plate 12 to move along the Y-axis in the forward direction, and when the Y-directional sensor 21 senses the Y-directional positioning plate 12, the sample clamping and moving device 2 stops moving, records the Y-directional coordinate, and returns to the initial position;
the sample clamping and moving device 2 clamps a sample to be detected, presses the sample analysis surface edge Z-direction positioning plate 14 or the sample analysis surface center Z-direction positioning column 13 to drive the sample analysis surface center Z-direction positioning plate 17 to move along the Z-axis negative direction; when the Z-direction sensor 18 at the center of the sample analysis surface senses the Z-direction positioning plate 17 at the center of the sample analysis surface, the sample clamping and moving device 2 stops moving, the size of the sample to be detected meets the requirement, the Z-direction coordinate is recorded, and then the subsequent detection steps S3-S8 are carried out; when the Z-direction sensor 15 senses the Z-direction positioning plate 14, the flatness of the analysis surface of the sample to be detected is determined not to meet the detection requirement, the sample to be detected is marked as a waste sample, and the process directly proceeds to step S8.
In step S4, the specific analysis process is as follows:
s4.1, the central control server 1 issues an instruction to the rare earth spectrum analyzer 7, and the sample number, the test times, the analysis curve and the sample brand are determined; the rare earth spectrum analyzer 7 informs the central control server 1 of confirming the instruction reception after receiving the instruction;
s4.2, the sample to be detected is conveyed to an analysis table of the rare earth spectrum analyzer 7 by the sample clamping and moving device 2, and after a groove of the sample to be detected is arranged on a boss of the analysis table of the rare earth spectrum analyzer 7, the analysis surface is in a closed argon atmosphere; the central control server 1 informs the rare earth spectrometer 7 of the preparation for analysis, and after the rare earth spectrometer 7 receives the instruction, the analysis is started and the central control server 7 is informed of the start of the analysis;
s4.3, the central control server 1 inquires whether the analysis of the rare earth spectrometer 7 is finished, and after the analysis is finished, the rare earth spectrometer 7 informs the central control server 1 that the analysis is finished;
s4.4, the central control server 1 receives the last analysis ending instruction, judges the excitation times, moves the sample point changing and carries out secondary analysis;
s4.5, the rare earth spectrometer 7 informs the central control server 1 that the secondary analysis is finished; after the central control server 1 receives the instruction, the central control server prepares to receive the analysis result data, and the rare earth spectrometer 7 sends the analysis result data to the central control server 1, wherein the analysis result data is the average value of the two analysis result data.
When the method is used for classifying praseodymium-neodymium based mixed rare earth metal samples, in the step S5, the detected rare earth elements and alloy elements are neodymium and praseodymium, and the impurity elements are carbon, iron, silicon, aluminum and molybdenum.
In the step S5, if the shape and size of the sample do not meet the requirements, the sample is directly classified into D and other products; for the sample with the shape and the size meeting the requirements, if the analysis result m (Fe) of the Fe element is more than 0.2 percent or the analysis result m (C) of the C element is more than 0.05 percent, classifying the sample into a C product and the like; if the analysis result m of the Fe element (Fe) is less than or equal to 0.2 percent and the analysis result m of the C element (C) is less than or equal to 0.03 percent, classifying the sample into A class and the like, otherwise, classifying the sample into B class and the like.
Compared with the prior art, the invention has the beneficial effects that:
the high-speed full-automatic spectral analysis and classification system for rare earth metals integrates sample processing, spectral analysis, sample weighing and automatic marking and classification, has high analysis speed, high accuracy and strong instantaneity, and finishes all actions within 3 minutes. Compared with the traditional ICP analysis method, the method aims at the sample with the rare earth element content of more than 50 wt%, and the solid sample is adopted for direct excitation analysis, so that the processes of chip-making sampling, dissolving, diluting and the like are omitted, the analysis error caused by sample dissolving and diluting is reduced, and the analysis precision of the high-content (>10 wt%) element is superior to the test result of the ICP method.
Compared with the rare earth spectrum analyzer 7 which is independently adopted in the prior art, the rare earth spectrum analyzer adopting the full-automatic analysis and classification system can integrate sample weighing, marking, sample preparation, analysis and classification, realizes high-speed automatic analysis, greatly improves the analysis efficiency, can avoid sample sampling inspection, and meets the technical requirement that sample blocks need to be inspected.
Drawings
FIG. 1 is a schematic perspective view of a high-speed full-automatic spectral analysis and classification system for rare earth metals;
fig. 2a is a schematic perspective view of the front surface of the analysis surface positioning device 5;
FIG. 2b is a schematic side view of the analysis surface positioning device 5;
FIG. 3 is a schematic view of a three-dimensional structure of a groove on the surface of a sample to be measured;
fig. 4 is a schematic perspective view of an analysis stage of the rare earth spectrum analyzer 7;
fig. 5 is a schematic perspective view of the analysis surface processing apparatus 6;
fig. 6 is a schematic perspective view of the automatic weighing device 8;
fig. 7 is a schematic perspective view of the automatic marking device 9;
FIG. 8 is a schematic perspective view of a finished product classification device;
FIG. 9 is a flow chart of the high-speed full-automatic spectral analysis and classification method for rare earth metals according to the present invention;
FIG. 10 is a schematic perspective view of a standard sample;
FIG. 11 is a flow chart of the rare earth spectroscopic analysis portion of the method of the present invention;
fig. 12 is a flowchart illustrating the classification in step S5 of the classification method according to the embodiment.
Wherein the reference numerals are:
1 Central control Server
2 sample clamping and moving device
3 sampling point
4 sample conveyer to be measured
5 analysis surface positioning device
6 analysis face processingequipment
7 rare earth spectrum analyzer
8 automatic weighing device
9 automatic marking device
10 finished product classification bin
11 sorting push rod
12Y-direction positioning plate
13 sample analysis face center Z is to reference column
14Z-direction positioning plate for edge of sample analysis surface
15 sample analysis face edge Z sensor
16Z-direction edge guide post
17Z-direction positioning plate for center of sample analysis surface
18 sample analysis surface center Z-direction sensor
19Z-direction central guide post
20Y guide post
21Y-direction sensor
Detailed Description
The present invention will be further explained with reference to the drawings and examples, which are used for classifying PrNd rare earth metal samples (rare earth element content greater than 99 wt%).
As shown in fig. 1, the high-speed full-automatic spectrum analysis and classification system for rare earth metals comprises a central control server 1, a sample clamping and moving device 2, a to-be-detected sample conveying device 4, an analysis surface positioning device 5, an analysis surface processing device 6, a rare earth spectrum analyzer 7, an automatic weighing device 8, an automatic marking device 9 and a finished product grading and classification device.
The sample clamping and moving device 2 adopts a high-precision numerical control system to accurately control the clamped sample to be detected to move in the horizontal X-axis direction, the Y-axis direction and the vertical Z-axis direction; the sample conveying device 4 to be tested, the analysis surface positioning device 5, the analysis surface processing device 6, the rare earth spectrum analyzer 7, the automatic weighing device 8, the automatic marking device 9 and the finished product grading and classifying device are sequentially arranged in parallel along the X-axis direction of the sample clamping and moving device 2.
The sample conveying device 4 is used for conveying the sample to be detected to the sampling point 3 of the sample clamping and moving device 2.
As shown in fig. 2a and 2b, the analysis surface positioning device 5 is used for determining the position of an analysis surface on a sample to be measured, and comprises an analysis surface positioning device housing, a Y-directional positioning plate 12, a Y-directional guide post 20, a Y-directional sensor 21, a sample analysis surface center Z-directional positioning post 13, a Z-directional edge guide post 16, a sample analysis surface center Z-directional positioning plate 17, a sample analysis surface center Z-directional sensor 18, a Z-directional center guide post 19, a sample analysis surface edge Z-directional positioning plate 14 and a sample analysis surface edge Z-directional sensor 15.
A pair of horizontally arranged Y-direction guiding columns 20 are slidably mounted on the analysis surface positioning device shell along the Y-axis direction, the positive Y-axis end of the Y-direction guiding column 20 positioned in the analysis surface positioning device shell is provided with a nut, and the Y-direction positioning plate 12 is vertically and fixedly connected with the negative Y-axis end of the Y-direction guiding column 20 positioned outside the analysis surface positioning device shell; a spring is provided on the Y-direction guide 20 between the Y-direction positioning plate 12 and the analysis surface positioning device housing, so that when the sample holding/moving device 2 holds the sample and pushes the Y-direction positioning plate 12 in the Y-axis forward direction, the Y-direction positioning plate 12 can move within a certain range, and the Y-direction positioning plate 12 can be returned to the original position after being moved away. The Y-direction sensor 21 is disposed between the Y-direction positioning plate 12 and the analysis surface positioning device housing, and is used for detecting whether the Y-direction positioning plate 12 moves to a limited position.
A pair of vertically arranged Z-direction edge guide posts 16 and a pair of vertically arranged Z-direction central guide posts 19 are slidably mounted on the analysis surface positioning device housing along the Z-axis direction, the Z-direction edge guide posts 16 and the Z-direction central guide posts 19 are mounted with nuts at the Z-axis negative ends inside the analysis surface positioning device housing, and the sample analysis surface edge Z-direction positioning plate 14 is horizontally and fixedly connected to the Z-axis positive ends of the Z-direction edge guide posts 16 outside the analysis surface positioning device housing; a spring is arranged on the Z-directional edge guide post 16 between the sample analysis surface edge Z-directional positioning plate 14 and the analysis surface positioning device housing, so that when the sample clamping movement device 2 clamps a sample and pushes the sample analysis surface edge Z-directional positioning plate 14 along the Z-axis negative direction, the sample analysis surface edge Z-directional positioning plate 14 can move within a certain range, and the sample analysis surface edge Z-directional positioning plate 14 can be restored to the original position after the sample is removed.
The sample analysis surface center Z-direction positioning plate 17 is horizontally and fixedly connected to the Z-axis positive end of the Z-direction center guide pillar 19 positioned outside the analysis surface positioning device shell, and the sample analysis surface center Z-direction positioning plate 17 is positioned below the sample analysis surface edge Z-direction positioning plate 14; the sample analysis surface center Z-direction positioning column 13 is vertically and fixedly connected to the middle of the sample analysis surface center Z-direction positioning plate 17, and the top end of the sample analysis surface center Z-direction positioning column 13 can freely slide upwards to penetrate through a through hole in the middle of the sample analysis surface edge Z-direction positioning plate 14 and protrude out of the surface of the sample analysis surface edge Z-direction positioning plate 14. A spring is arranged on a Z-direction central guide pillar 19 between the sample analysis surface center Z-direction positioning plate 17 and the analysis surface positioning device shell, when the sample clamping moving device 2 clamps a sample and pushes the sample analysis surface center Z-direction positioning column 13 along the Z-axis negative direction, the sample analysis surface center Z-direction positioning plate 17 can move in a certain range, and after the sample is removed, the sample analysis surface center Z-direction positioning plate 17 and the sample analysis surface center Z-direction positioning column 13 can restore to the original positions. The sample analysis surface edge Z-direction sensor 15 is positioned below the sample analysis surface edge Z-direction positioning plate 14, and the sample analysis surface center Z-direction sensor 18 is positioned below the sample analysis surface center Z-direction positioning plate 17 and is higher than the sample analysis surface edge Z-direction sensor 15.
The analysis surface processing device 6 is used for processing a groove on the analysis surface position of the sample to be detected, which is determined by the analysis surface positioning device 5, and processing a flat analysis surface in the groove, as shown in fig. 3, wherein the groove width d is 35 mm. The shape of the groove is matched with the shape of a boss on an analysis table of the rare earth spectrum analyzer 7, and as shown in fig. 4, the boss is 30mm wide, so that after a sample to be detected is installed on the analysis table of the rare earth spectrum analyzer 7, the analysis surface is in a closed argon atmosphere.
As shown in fig. 5, metal protective covers are installed around and on the analysis surface processing device 6 to prevent metal scraps from splashing in the processing process, and an opening is formed in one end of each metal protective cover to facilitate the sample clamping and moving device 2 to clamp the sample to be detected to enter and exit.
The rare earth spectrum analyzer 7 realizes automatic electrode brushing, automatic regular internal standard calibration, automatic curve height calibration, classification of samples to be detected according to set component content classification rules, and storage of sample analysis results in a database of the central control server 1.
As shown in fig. 6, the automatic weighing device 8 is used for weighing the measured sample and transmitting the weight of the sample to the database of the central control server 1 for storage.
As shown in fig. 7, the automatic marking device 9 is configured to mark a sample number at a designated position of a measured sample by physical imprinting, and store the sample number in a database of the central control server 1. The sample marking method is not limited to a physical stamping method, and includes laser marking, pneumatic marking, surface printing and the like.
As shown in fig. 8, the finished product classifying device includes a finished product conveyor belt, a classifying push rod 11, and a plurality of finished product classifying bins 10. Be equipped with the finished product platform on the conveyer belt, categorised push rod 11 sets up on the finished product platform, can push the sample into corresponding finished product classification storehouse 10 according to central control server 1's instruction.
The central control server 1 is respectively connected with the sample clamping and moving device 2, the sample conveying device 4 to be tested, the analysis surface positioning device 5, the analysis surface processing device 6, the rare earth spectrum analyzer 7, the automatic weighing device 8, the automatic marking device 9 and the finished product classification device, the sample clamping and moving device 2 is controlled to clamp the sample to be tested conveyed by the sample conveying device 4 to be tested from the sampling point 3, the sample to be tested is sequentially processed by the analysis surface positioning device 5, the analysis surface processing device 6, the rare earth spectrum analyzer 7, the automatic weighing device 8 and the automatic marking device 9 and then is placed on a conveying belt 10, and according to the classification result of the rare earth spectrum analyzer 7, after the sample moves to the corresponding position of the finished product classification bin 10 on the finished product conveying belt, the classification and classification of the sample are realized by the classification push rods 11.
As shown in fig. 9, the high-speed full-automatic spectral analysis method for rare earth metals of the present invention comprises the following steps:
s1, transferring and clamping the sample;
after cooling down (the temperature of the sample is less than 40 ℃) a rare earth metal sample to be tested (shown in figure 10) which is cast into a fixed pattern by using a sampling mold, placing the rare earth metal sample to be tested on a sample conveying device 4 to be tested, moving the sample to be tested to a sampling point 3 by the sample conveying device 4 to be tested, and controlling a sample clamping movement device 2 to clamp the sample to be tested by a central control server 1;
s2, determining the analysis position;
the sample holding and moving device 2 moves the sample to be measured to the analysis surface positioning device 5 to determine the position of the analysis surface of the sample to be measured.
The sample clamping and moving device 2 clamps a sample to be measured, presses the Y-direction positioning plate 12 to move along the Y-axis forward direction, and when the Y-direction sensor 21 senses the Y-direction positioning plate 12, the sample clamping and moving device 2 stops moving, records the Y-direction coordinate and returns to the initial position.
The sample clamping and moving device 2 clamps a sample to be detected, presses the edge Z-direction positioning plate 14 of the sample analysis surface or the center Z-direction positioning column 13 of the sample analysis surface to drive the center Z-direction positioning plate 17 of the sample analysis surface to move along the Z-axis in the negative direction. When the sample analysis surface center Z-direction sensor 18 senses the sample analysis surface center Z-direction positioning plate 17, the sample clamping movement device 2 stops moving, the size of the sample to be detected meets the requirement, the Z-direction coordinate is recorded, and the subsequent detection steps S3-S8 can be carried out; when the sample analysis surface edge Z-direction sensor 15 senses the sample analysis surface edge Z-direction positioning plate 14, it is determined that the flatness of the analysis surface of the sample to be detected does not meet the detection requirement, the sample to be detected is marked as a waste sample, and the process directly enters step S8;
s3, analyzing surface processing;
sample centre gripping telecontrol equipment 2 will await measuring the sample and remove to analysis face processingequipment 6, and analysis face processingequipment drives milling cutter rotation machining sample analysis face for the motor, processes a recess on the analysis surface position that analysis face positioner 5 confirmed, and process smooth analysis surface in the recess, the shape of recess and the boss shape phase-match on the analysis bench of rare earth spectral analyzer 7 guarantee the gas tightness among the analytic process.
S4, spectral analysis;
as shown in fig. 11, the specific analysis process is as follows:
and S4.1, the central control server 1 issues an instruction to the rare earth spectrum analyzer 7, and a sample number (00000001), a test frequency (2), an analysis curve (praseodymium-neodymium alloy) and a sample number (7525) are determined. The rare earth spectrum analyzer 7 notifies the central control server 1 of the confirmation of the instruction reception after receiving the instruction.
S4.2, the sample to be detected is conveyed to an analysis table of the rare earth spectrum analyzer 7 by the sample clamping and moving device 2, and after a groove of the sample to be detected is arranged on a boss of the analysis table of the rare earth spectrum analyzer 7, the analysis surface is in a closed argon atmosphere; the central control server 1 informs the rare earth spectrometer 7 of the preparation for analysis, and after receiving the instruction, the rare earth spectrometer 7 starts the analysis and informs the central control server 7 of the start of the analysis.
And S4.3, the central control server 1 inquires whether the analysis of the rare earth spectrometer 7 is finished or not, and after the analysis is finished, the rare earth spectrometer 7 informs the central control server 1 that the analysis is finished.
And S4.4, the central control server 1 receives the last analysis ending instruction, judges the excitation times (2 times), moves the sample point changing and carries out secondary analysis.
And S4.5, the rare earth spectrometer 7 informs the central control server 1 of the end of the secondary analysis. After the central control server 1 receives the instruction, the central control server prepares to receive the analysis result data, and the rare earth spectrometer 7 sends the analysis result data to the central control server 1, wherein the analysis result data is the average value of the two analysis result data, and the analysis result is shown in table 1.
Table 1 example analytical results data
S5, classifying;
the rare earth spectrum analyzer 7 classifies according to the shape and size of the sample and the analysis result of C, Fe elements, as shown in fig. 12, the specific process is as follows: if the shape and the size of the sample do not meet the requirements, directly classifying the sample into D and other products; classifying the sample with the shape and the size meeting the requirement into a C grade product if the analysis result m (Fe) of the Fe element is more than 0.2 percent or the analysis result m (C) of the C element is more than 0.05 percent; if the analysis result m of the Fe element (Fe) is less than or equal to 0.2 percent and the analysis result m of the C element (C) is less than or equal to 0.03 percent, classifying the sample into A class and the like, otherwise, classifying the sample into B class and the like. The rare earth spectrum analyzer 7 transmits the analysis result data, classification level and sample number to the database of the central control server 1.
S6, weighing;
the sample gripping and movement device 2 moves the sample from the analysis station to the automatic weighing device 8, deposits the sample, weighs, transmits the weight data (6kg) to the database of the central control server 1 and matches the corresponding number. And (5) grabbing the sample for the second time.
S7, the sample holding/moving device 2 moves the sample to the automatic marking device 9, and the sample surface is marked with the sample number (00000001).
And S8, the sample clamping and moving device 2 moves the sample to the finished product conveyor belt. According to the classification result, the classification push rod 11 ejects the sample from the conveyor belt to the finished product classification bin 10.
The complete analysis process of one sample takes 2 minutes and 47 seconds, the analysis result is accurate, and a very good application effect is obtained.
Claims (12)
1. A rare earth metal high-speed full-automatic spectrum analysis and classification system is characterized by comprising a central control server (1), a sample clamping and moving device (2), a to-be-detected sample conveying device (4), an analysis surface positioning device (5), an analysis surface processing device (6), a rare earth spectrum analyzer (7), an automatic weighing device (8), an automatic marking device (9) and a finished product grading and classification device, wherein the content of rare earth elements in a sample is more than 50%;
the sample clamping and moving device (2) adopts a high-precision numerical control system to accurately control the clamped sample to be tested to move in the horizontal X-axis direction, the Y-axis direction and the vertical Z-axis direction; the sample conveying device (4) to be tested, the analysis surface positioning device (5), the analysis surface processing device (6), the rare earth spectrum analyzer (7), the automatic weighing device (8), the automatic marking device (9) and the finished product grading and classifying device are sequentially arranged in parallel along the X-axis direction of the sample clamping and moving device (2);
the to-be-detected sample conveying device (4) is used for conveying a to-be-detected sample to the sampling point (3) of the sample clamping and moving device (2);
the analysis surface positioning device (5) is used for determining the position of an analysis surface on a sample to be detected;
the analysis surface processing device (6) is used for processing a groove on the analysis surface position of the sample to be detected, which is determined by the analysis surface positioning device (5), and processing a flat analysis surface in the groove, wherein the shape of the groove is matched with the shape of a boss on an analysis table of the rare earth spectrum analyzer (7), so that after the sample to be detected is arranged on the analysis table of the rare earth spectrum analyzer (7), the analysis surface is in a closed argon atmosphere;
the rare earth spectrum analyzer (7) realizes automatic electrode brushing, automatic regular internal standard calibration and automatic curve high-low standard calibration, samples to be detected are classified according to set component content classification rules, and sample analysis results are stored in a database of the central control server (1);
the automatic weighing device (8) is used for weighing the measured sample and transmitting the weight of the sample to a database of the central control server (1) for storage;
the automatic marking device (9) is used for marking a sample number at the specified position of a measured sample and storing the sample number into a database of the central control server (1);
the finished product grading and classifying device comprises a finished product conveyor belt, a classifying push rod (11) and a plurality of finished product classifying bins (10); a finished product platform is arranged on the finished product conveyor belt, and the classification push rod (11) is arranged on the finished product platform and can push the samples into corresponding finished product classification bins (10) according to the instruction of the central control server (1);
the analysis surface positioning device (5) comprises two fixing plates which are vertical to each other, and a Y-direction positioning plate (12) and two Z-direction positioning plates which can move samples along the Y-axis direction and the Z-axis direction are respectively installed on the fixing plates, each positioning plate is provided with a corresponding sensor, the positioning plates are supported by a plurality of guide pillars, and each guide pillar is sleeved with a return spring; the two Z-direction positioning plates are a sample analysis surface edge Z-direction positioning plate (14) and a sample analysis surface center Z-direction positioning plate (17), are arranged in parallel, and are matched with the sensor to judge whether the sample is a waste sample;
the analysis surface positioning device (5) further comprises: the analysis surface positioning device comprises a shell provided with two fixing plates, a Y-direction guide post (20), a Y-direction sensor (21), a sample analysis surface center Z-direction positioning post (13), a Z-direction edge guide post (16), a sample analysis surface center Z-direction sensor (18), a Z-direction center guide post (19) and a sample analysis surface edge Z-direction sensor (15); wherein:
a pair of horizontally arranged Y-direction guide posts (20) is slidably mounted on the shell of the analysis surface positioning device along the Y-axis direction, the positive ends of the Y-direction guide posts (20) positioned in the shell of the analysis surface positioning device are provided with nuts, and the Y-direction positioning plate (12) is vertically and fixedly connected with the negative ends of the Y-direction guide posts (20) positioned outside the shell of the analysis surface positioning device; a return spring is arranged on the Y-direction guide post (20) between the Y-direction positioning plate (12) and the shell of the analysis surface positioning device; the Y-direction sensor (21) is arranged between the Y-direction positioning plate (12) and the shell of the analysis surface positioning device and is used for detecting whether the Y-direction positioning plate (12) moves to a limited position or not;
a pair of vertically arranged Z-direction marginal guide posts (16) and a pair of vertically arranged Z-direction central guide posts (19) are slidably arranged on the shell of the analysis surface positioning device along the Z-axis direction, the Z-direction marginal guide posts (16) and the Z-direction central guide posts (19) are arranged at the Z-axis negative ends positioned in the shell of the analysis surface positioning device and are provided with nuts, and the sample analysis surface marginal Z-direction positioning plate (14) is horizontally and fixedly connected at the Z-axis positive end of the Z-direction marginal guide posts (16) positioned outside the shell of the analysis surface positioning device; a return spring is arranged on a Z-direction edge guide post (16) between the Z-direction positioning plate (14) at the edge of the sample analysis surface and the shell of the analysis surface positioning device;
the sample analysis surface center Z-direction positioning plate (17) is horizontally and fixedly connected to the Z-axis forward end, located outside the analysis surface positioning device shell, of the Z-direction center guide pillar (19), and the sample analysis surface center Z-direction positioning plate (17) is located below the sample analysis surface edge Z-direction positioning plate (14); the center Z-direction positioning column (13) of the sample analysis surface is vertically and fixedly connected to the middle part of the center Z-direction positioning plate (17) of the sample analysis surface, and the top end of the center Z-direction positioning column (13) of the sample analysis surface can upwards freely slide through a through hole in the middle part of the edge Z-direction positioning plate (14) of the sample analysis surface and protrude out of the surface of the edge Z-direction positioning plate (14) of the sample analysis surface; a return spring is arranged on a Z-direction central guide post (19) between the Z-direction positioning plate (17) of the sample analysis surface center and the analysis surface positioning device shell; the Z-direction sensor (15) at the edge of the sample analysis surface is positioned below the Z-direction positioning plate (14) at the edge of the sample analysis surface, and the Z-direction sensor (18) at the center of the sample analysis surface is positioned below the Z-direction positioning plate (17) at the center of the sample analysis surface and is higher than the Z-direction sensor (15) at the edge of the sample analysis surface.
2. The high-speed full-automatic spectral analysis and classification system for rare earth metals according to claim 1, wherein the analysis surface processing device (6) is a milling cutter driven by a motor to rotate and process the analysis surface of the sample.
3. The high-speed full-automatic spectral analysis and classification system for rare earth metals according to claim 1, wherein metal protective covers are installed around and above the analysis surface processing device (6) to prevent metal chips from splashing during processing, and an opening is formed at one end of each metal protective cover to facilitate the sample to be detected to be clamped by the sample clamping and moving device (2) to enter and exit.
4. The high-speed full-automatic spectral analysis and classification system for rare earth metals according to claim 1, wherein the sample marking method of the automatic marking device (9) comprises physical imprinting, laser marking, pneumatic marking and surface printing.
5. The high-speed full-automatic spectral analysis and classification system for rare earth metals according to claim 1, wherein the time for full-process analysis of each sample is less than 3 minutes.
6. The high-speed full-automatic spectral analysis and classification system for rare earth metals according to claim 1, wherein the rare earth metals are single rare earth metals, mixed rare earth metals or rare earth alloys with more than 50% of rare earth elements.
7. A method for high-speed full-automatic spectroscopic analysis and classification of rare earth metals according to the system of claims 1-6, wherein the method comprises the steps of:
s1, sample conveying and clamping:
after cooling down a rare earth metal to-be-detected sample which is cast into a fixed pattern by using a sampling mold, placing the rare earth metal to-be-detected sample on a to-be-detected sample conveying device (4), moving the to-be-detected sample to a sampling point (3) by using the to-be-detected sample conveying device (4), and controlling a sample clamping movement device (2) to clamp the to-be-detected sample by using a central control server (1);
s2, analyzing the position determination and judging the waste sample:
the sample clamping and moving device (2) moves the sample to be detected to the analysis surface positioning device (5) so as to determine the analysis surface position of the sample to be detected and judge whether the sample to be detected is a waste sample;
s3, analyzing surface processing:
the sample clamping and moving device (2) moves a sample to be tested to the analysis surface processing device (6), a groove is processed on the analysis surface position determined by the analysis surface positioning device (5), a flat analysis surface is processed in the groove, the shape of the groove is matched with the shape of a boss on an analysis table of the rare earth spectrum analyzer (7), and the air tightness in the analysis process is guaranteed;
s4, spectral analysis;
s5, classification:
the rare earth spectrum analyzer (7) classifies according to the shape and size of the sample and the analysis results of the rare earth elements, the alloy elements and the impurity elements, and transmits the analysis result data, classification grade and sample number to a database of the central control server (1);
s6, weighing:
the sample clamping and moving device (2) moves the sample to an automatic weighing device (8) from an analysis table of the rare earth spectrum analyzer (7), puts down the sample, weighs, transmits weight data to a database of the central control server (1), and matches the weight data with a corresponding serial number; grabbing a sample for the second time;
s7, moving the sample to an automatic marking device (9) by the sample clamping and moving device (2), and marking a sample number at a designated position on the surface of the sample;
s8, the sample is moved to a finished product table of the finished product conveyor belt by the sample clamping and moving device (2), and the samples are ejected out of the conveyor belt to a finished product sorting bin (10) by the sorting push rod (11) according to a sorting result.
8. The method according to claim 7, wherein in step S1, the sample temperature is <40 ℃.
9. The method according to claim 7, wherein in step S2, the sample holding and moving device (2) holds the sample to be tested and presses the Y-positioning plate (12) to move along the Y-axis in the forward direction, when the Y-positioning plate (12) is sensed by the Y-sensor (21), the sample holding and moving device (2) stops moving, records the Y-coordinate and returns to the initial position;
the sample clamping and moving device (2) clamps a sample to be detected, presses the edge Z-direction positioning plate (14) of the sample analysis surface or the center Z-direction positioning column (13) of the sample analysis surface to drive the center Z-direction positioning plate (17) of the sample analysis surface to move along the Z-axis in the negative direction; when the Z-direction sensor (18) at the center of the sample analysis surface senses the Z-direction positioning plate (17) at the center of the sample analysis surface, the sample clamping and moving device (2) stops moving, the size of a sample to be detected meets the requirement, Z-direction coordinates are recorded, and then the subsequent detection steps S3-S8 are carried out; when the Z-direction sensor (15) at the edge of the sample analysis surface senses the Z-direction positioning plate (14) at the edge of the sample analysis surface, the flatness of the analysis surface of the sample to be detected is judged not to meet the detection requirement, the sample to be detected is marked as a waste sample, and the step S8 is directly carried out.
10. The method according to claim 7, wherein in the step S4, the specific analysis process is as follows:
s4.1, the central control server (1) issues an instruction to the rare earth spectrum analyzer (7) to determine a sample number, test times, an analysis curve and a sample brand; the rare earth spectrum analyzer (7) informs the central control server (1) of confirming the instruction receipt after receiving the instruction;
s4.2, the sample to be detected is conveyed to an analysis table of the rare earth spectrum analyzer (7) by the sample clamping and moving device (2), and after a groove of the sample to be detected is arranged on a boss of the analysis table of the rare earth spectrum analyzer (7), the analysis surface is in a closed argon atmosphere; the central control server (1) informs the rare earth spectrometer (7) of the preparation for analysis, and after the rare earth spectrometer (7) receives the instruction, the analysis is started and the central control server (1) is informed of the start of the analysis;
s4.3, the central control server (1) inquires whether the analysis of the rare earth spectrometer (7) is finished, and after the analysis is finished, the rare earth spectrometer (7) informs the central control server (1) that the analysis is finished;
s4.4, the central control server (1) receives the last analysis ending instruction, judges the excitation times, moves the sample point changing and carries out secondary analysis;
s4.5, the rare earth spectrometer (7) informs the central control server (1) that the secondary analysis is finished; after the central control server (1) receives the instruction, the central control server prepares to receive the analysis result data, and the rare earth spectrometer (7) sends the analysis result data to the central control server (1), wherein the analysis result data is the average value of the two analysis result data.
11. The method according to claim 7, wherein when the method is used for classifying praseodymium-neodymium based mixed rare earth metal samples, in the step S5, the rare earth elements and alloy elements detected are neodymium and praseodymium, and the impurity elements are carbon, iron, silicon, aluminum and molybdenum.
12. The method according to claim 11, wherein in step S5, if the shape and size of the sample do not meet the requirement, the sample is directly classified into D class; classifying the sample with the shape and the size meeting the requirement into a C grade product if the analysis result m (Fe) of the Fe element is more than 0.2 percent or the analysis result m (C) of the C element is more than 0.05 percent; if the analysis result m of the Fe element (Fe) is less than or equal to 0.2 percent and the analysis result m of the C element (C) is less than or equal to 0.03 percent, classifying the sample into A class and the like, otherwise, classifying the sample into B class and the like.
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