CN115828574B - Plasma spraying parameter determination method - Google Patents

Plasma spraying parameter determination method Download PDF

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CN115828574B
CN115828574B CN202211503716.4A CN202211503716A CN115828574B CN 115828574 B CN115828574 B CN 115828574B CN 202211503716 A CN202211503716 A CN 202211503716A CN 115828574 B CN115828574 B CN 115828574B
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factor
ctr
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parameter
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CN115828574A (en
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朱文健
顾鹏铭
徐国俊
顾仁宝
李伟东
周宇伟
刘兴明
韩伟男
薛弘宇
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Jiangsu Kaiweites Semiconductor Technology Co ltd
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Jiangsu Kaiweites Semiconductor Technology Co ltd
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Abstract

The invention discloses a plasma spraying parameter determining method, which belongs to the technical field of computers, wherein the method comprises the steps of sequentially determining and optimizing spraying parameters by using multiple stages, and the method can be used for finding the optimal parameters in a plasma spraying parameter data test, reducing the corrosion influence degree of a plasma etching process by reducing the test times of etching rate, ensuring the test quality, avoiding missing important influence factors, and solving the problems that a short plate of a traditional orthogonal test is only limited to the optimal combination of factor levels, is a region with a larger range and cannot really find the optimal parameters of equipment.

Description

Plasma spraying parameter determination method
Technical Field
The invention belongs to the technical field of computers, and particularly relates to a plasma spraying parameter determination method.
Background
The reaction gases for plasma etching comprise CF4/O2, NF3, cl2, CH4/Ar and the like, a large amount of active free radicals such as Cl radicals, F radicals and the like can be generated in the dry etching process of the plasma, and can generate corrosion effect on the inner surface of a plasma etching process cavity prepared by aluminum and aluminum alloy when the semiconductor device is etched, and a large amount of particles are generated by the strong corrosion, so that frequent maintenance of production equipment is required, and even the failure of the etching process cavity and the damage of the device can be caused in serious cases.
With the development of thermal spray technology, in particular plasma spray technology, and the diversification of ceramic materials, it has not only solved the corrosion problem of plasma etching process chambers technically but also economically. However, as the size of the wafer increases, the inner diameter of the plasma etching process cavity has increased from 400mm to 500-600 mm, and the corresponding plasma power also increases, so that the porosity and the binding force of the equipment to the ceramic coating are higher and higher.
Ceramic coating properties are affected by a number of factors in the spray equipment, such as: powder feeding argon, powder feeding amount, current, main argon, hydrogen and the like, and the physicochemical properties of spray powder are as follows: particle size, density, sphericity, etc. Comprehensive systematic experiments are carried out on all the factors to explore the corresponding influence, so that a large amount of experimental work is necessarily faced, a large amount of working hours and material consumption are generated, and the conditions are limited. Therefore, a scientific experiment design method is needed, a set of scientific and efficient experiment analysis method is designed by combining the practical spraying operation, experimental data results are needed to meet the practical requirements of production demands, and meanwhile, the corrosion problem of a plasma etching process can be reduced as much as possible.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a plasma spraying parameter determining method, which comprises the following steps:
step S1, determining test factors, factor levels and test indexes of a first stage of plasma spraying test, wherein the test factors comprise powder feeding argon A1, powder feeding quantity A2, current A3, main argon A4, hydrogen A5, spraying interval A6 and rotating disc rotating speed A7, the test indexes comprise porosity C1, bonding strength C2, hardness C3 and dielectric constant C4 of the coating, and the factor levels are that 3 levels are selected from seven test factors represented by the A1-A7 in a range supported by test equipment;
step S2, determining an orthogonal test table and determining a test scheme, wherein the test scheme comprises test factors and combination of factor levels, and is expressed asWhere k=1, 2,..7, l=1, 2,3, indicating that Ak represents the experimental factor takes on value at level L;
step S3, testing according to the orthogonal test table, and measuring the porosity C1, the bonding strength C2, the hardness C3 and the dielectric constant C4 of the coating;
step S4, calculating a single factor contribution rate of powder feeding argon A1, powder feeding quantity A2, current A3, main argon A4, hydrogen A5, spraying interval A6 and rotating disc rotating speed A7 to porosity C1, bonding strength C2, hardness C3 and dielectric constant C4;
step S5, determining a comprehensive contribution rate according to the single factor contribution rate, and determining test factors corresponding to the comprehensive contribution rate exceeding a decision threshold and corresponding factor levels of the comprehensive contribution rate exceeding the decision threshold as test parameter values of the first-stage test when the comprehensive contribution rate exceeds the decision threshold of a single test index, wherein the test parameter values are n items;
s6, determining default test factors of seven test factors represented by A1-A7 in test parameter values tested in the first stage, determining default test indexes of four test indexes represented by C1-C4 in single test indexes with up-to-standard comprehensive contribution rates, and determining (7-n) default test factors;
step S7, determining test factors, factor levels and test indexes of a plasma spraying second stage test, wherein the test factors comprise seven test factors represented by A1-A7, the test factors comprise (7-n) default test factors and test parameter values of the first stage test of which the values are determined in the first stage test, the test indexes also comprise etching rate C0, the factor levels are 3 levels selected from (7-n) test factors represented by (7-n) default test factors in the range supported by corresponding test equipment, and n parameter combinations are randomly selected, and the test parameter values of the test factors in the parameter combinations are different from the test parameter values of the first stage test which are determined;
step S8, determining a numerical relation model between the etching rate C0 and seven test factors represented by A1-A7Obtaining m by linear fitting k A value of (k=1, 2, …, 7);
step S9, removing the n test parameter values of the determined first stage test, comprehensively sequencing the rest (7-n) test factors to obtain the optimal factor level of each of the rest (7-n) test factors, and determining the theoretical optimal process parameter level P1-P7 of the test factors by combining the test parameter values of the first stage test;
step S10, determining an optimal process parameter interval corresponding to the optimal process parameter level of each test factor according to the step S9;
step S11, uniformly sampling in the optimal process parameter interval corresponding to the optimal process parameter level of each factor, selecting w sampling points, and generating all experimental combinations determined by the optimal process parameters, wherein the experimental combinations comprise w 7 A combination of items;
step S12, for the w 7 Obtaining a value of a predicted etching rate by using the numerical relation model f (C0) determined in the step S9, and measuring the porosity C1, the bonding strength C2, the hardness C3 and the dielectric constant C4 of the coating;
step S13, for w 7 And comprehensively sequencing the term combinations, determining the top-ranked X term parameter combinations, measuring the etching rate C0 of the X term parameter combination samples, and determining the parameter combinations of the optimal samples as final plasma spraying parameters.
The calculating method of the single factor contribution rate in the step S4 includes:
calculate eachCorresponding individual contribution->Wherein the factor level corresponding to l=1 is lowest, the factor level corresponding to l=3 is highest, and the factor level corresponding to l=2 is located in the middle of the two.
For the followingThe Cd-th measurement mean of (2) is expressed as +.>Wherein d=1, 2,3,4, the measurement mean is the mean of all cds with Ak at factor level L;
for the case of l=1,the single contribution rate of (2) is calculated as follows:
for the case of l=2,the single contribution rate of (2) is calculated as follows:
for the purpose of l=3,the single contribution rate of (2) is calculated as follows:
in the step S5, a comprehensive contribution rate is determined according to the single factor contribution rate, which specifically includes: determination of
wherein Ctropt (T Ak ) Is thatThe optimal item in (2) is recorded as the Ctr corresponding factor level opt (T Ak ) Is added to the information;
for any Cd (d=1, 2,3, 4), ctr is determined opt (T Ak ) (k=1, 2,..7), and determining the optimal term combination [ Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj )]。
wherein ,Ctropt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Is Ctr opt (T Ak ) (k=1, 2,..7) the same absolute value as the optimization target direction, and recording the single factor contribution ranking order;
calculating the comprehensive contribution rate:
Ctr_ALL opt (Cd)=Ctr opt ′(T Ah )+Ctr opt ′(T Ai )+Ctr opt ′(T Aj )。
when Ctr opt ′(T Ah ),Ctr opt ′(T Ai ) Or Ctr opt ′(T Aj ) C1 is Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Take a negative value.
Ctr for C2-C4 opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Is the original value of (2).
wherein ,Ctropt (T Ak ) Is thatThe optimal term in (a) isOr minimum value of (1), wherein: the optimal term of the porosity C1 corresponds to the minimum term; the optimal term of the bonding strength C2 corresponds to the maximum value term; the optimal term of the hardness C3 corresponds to the maximum value term; the optimum term for the dielectric constant C4 corresponds to the maximum term.
When the comprehensive contribution rate exceeds the decision threshold value of the single test index, determining the test factors corresponding to the comprehensive contribution rate exceeding the decision threshold value and the corresponding factor level as the test parameter values of the first-stage test, wherein the method comprises the following steps:
when the comprehensive contribution rate ctr_all opt (Cd)≥Threshold deter At the time, ctr_all is determined opt (Cd) corresponding Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) The factor level as the additional information is taken as the factor level of the corresponding test factor.
Wherein when different comprehensive contribution rates Ctr_ALL exist opt (Cd) is greater than the decision threshold, but when there is a conflict in the factor levels of the determined test factors, determining the test parameter values for the first stage test according to the following rules:
step S51, when the determined factor levels of the test factors have conflicts, judging the Ctr corresponding to each factor level opt The single factor contribution rank of the value in the optimal item combination, and the factor level of the top rank is determined as the test parameter value of the test factor tested in the first stage;
step S52, when the ranking of the two is the same, determining the Ctr opt The factor level corresponding to the term with the greatest absolute value of the value is determined as the test parameter value for the test factor tested in the first stage.
In the step S9, the remaining (7-n) test factors are comprehensively ranked to obtain an optimal factor level of each of the remaining (7-n) test factors, and theoretical optimal process parameter levels P1-P7 of the test factors are determined by combining the test parameter values tested in the first stage, including: for each of the remaining (7-n) test factors, calculating the comprehensive change rate of the test index for C0-C4 under each factor level, and when the comprehensive change rate is the optimization result, determining the factor level corresponding to the optimization result as the optimal factor level of the test factor until the optimal factor level of each of the remaining (7-n) test factors is determined, and determining the theoretical optimal process parameter level P1-P7 of the test factor in combination with the test parameter value tested in the first stage.
The calculation mode of the comprehensive change rate is as follows:
for each test factor of the remaining (7-n) items, each item is calculatedThe single contribution rate of the corresponding test index +.>d=0, 1,2,3,4, calculating the term +.>Corresponding comprehensive rate of change->
wherein ,the single contribution rate of the test index Cd is determined under the condition that the test factor Ak is at the factor level L;
the optimal factor level corresponding to Ak is determined as follows:the max () function indicates a maximum function; determining the optimum factor level of the remaining (7-n) items in combination with the test parameter values of the first stage testTheoretical optimum process parameter levels P1-P7, which determine the factor level of the test factors.
In the step S10, an optimal process parameter interval corresponding to the optimal process parameter level of each test factor is determined according to the step S9.
The method comprises the following steps: the optimal process parameter interval is 5% of the range supported by the floating test equipment above and below the optimal process parameter level P1-P7 for each test factor.
I.e. [ Pk-R ] k *5%,Pk+R k *5%](k=1, 2,..7), wherein R k And (5) supporting a test total range for the test equipment corresponding to the kth test factor.
Wherein, in step S13, for w 7 Comprehensively sequencing the term combinations, determining X term parameter combinations with top ranking, measuring the etching rate C0 of the X term parameter combination samples, and determining the parameter combination of the optimal sample as a final plasma spraying parameter, wherein the method specifically comprises the following steps:
step s13_1, calculate w 7 Comprehensive ordering of item combinations:
for each combination of test factors Ak and the sampled value of the corresponding sampled point wCalculate each item +.>The single contribution rate of the corresponding test index Cd +.>Calculate the item +.>Corresponding estimated integrated change rate->
wherein ,d=1, 2,3,4 is the single contribution determined from the measurement of C1-C4,/v>d=0 is a single contribution rate determined by obtaining a value of the predicted etching rate using the numerical relation model f (C0) determined in step S9;
step s13_2, determiningThe top X parameter combination samples are used for carrying out etching rate C0 measurement to obtain a measured value VL of C0-C4 of each sample in the X parameter combination samples C0 -VL C4 An optimized evaluation value TVL for each sample is calculated, tvl=vl C4 +VL C3 +VL C2 -VL C1 -VL C0 The method comprises the steps of carrying out a first treatment on the surface of the And step S13-3, combining parameters of the sample with the maximum TVL value as final plasma spraying parameters.
Compared with the prior art, the method provided by the invention has the advantages that the optimal parameters are found in the plasma spraying parameter data test, the corrosion influence degree of the plasma etching process is reduced by reducing the test times of the etching rate, the spraying effect is better, the efficiency is higher, and the spraying quality is higher. The test quality can be ensured, important influencing factors are avoided, the test time can be saved, meanwhile, the short plate of the traditional orthogonal experiment is made up, the optimal parameters of the orthogonal experiment are limited to the optimal combination of factor levels, and the method is a section with a larger range and can not really find the optimal parameters of equipment.
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The above, as well as additional purposes, features, and advantages of exemplary embodiments of the present disclosure will become readily apparent from the following detailed description when read in conjunction with the accompanying drawings. Several embodiments of the present disclosure are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which like reference numerals refer to similar or corresponding parts and in which:
fig. 1 is a flowchart illustrating a plasma spray parameter determination method according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise, the "plurality" generally includes at least two.
It should be understood that although the terms first, second, third, etc. may be used to describe … … in embodiments of the present invention, these … … should not be limited to these terms. These terms are only used to distinguish … …. For example, the first … … may also be referred to as the second … …, and similarly the second … … may also be referred to as the first … …, without departing from the scope of embodiments of the present invention.
It should be understood that the term "and/or" as used herein is merely one relationship describing the association of the associated objects, meaning that there may be three relationships, e.g., a and/or B, may represent: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
The words "if", as used herein, may be interpreted as "at … …" or "at … …" or "in response to a determination" or "in response to a detection", depending on the context. Similarly, the phrase "if determined" or "if detected (stated condition or event)" may be interpreted as "when determined" or "in response to determination" or "when detected (stated condition or event)" or "in response to detection (stated condition or event), depending on the context.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a product or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such product or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a commodity or device comprising such element.
Alternative embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the invention discloses a method for determining plasma spraying parameters, which comprises the following steps:
step S1, determining test factors, factor levels and test indexes of a first stage of plasma spraying test, wherein the test factors comprise powder feeding argon A1, powder feeding quantity A2, current A3, main argon A4, hydrogen A5, spraying interval A6 and rotating disc rotating speed A7, the test indexes comprise porosity C1, bonding strength C2, hardness C3 and dielectric constant C4 of the coating, and the factor levels are that 3 levels are selected from seven test factors represented by the A1-A7 in a range supported by test equipment;
the matrix material is 6061 aluminum, and the matrix material is square sample with the size of 15 x 5mm and25 x 5mm round samples. Before plasma spraying coating, the base material is subjected to sand blasting pretreatment, and the surface roughness Ra is controlled to be 6-7 mu m. The powder material used for preparing the coating is produced by the Nippon Xinyue chemical industry Co., ltd, wherein the purity of the Y2O3 powder is 99.99%; Y2O3 in YAG accounts for 54-60%, al2O3 accounts for 40-46%; YF3 accounts for 99.9%. Spray for experimentsThe coating apparatus was a unicoat pro atmospheric plasma spray apparatus manufactured by Oerlikon Metco company, switzerland. The changing factors are powder feeding argon, powder feeding quantity, current, rotating speed of a rotating disc, main argon, hydrogen and spraying interval, and 3 proper levels are selected from 7 factors in the range supported by the equipment. The preparation process of the test sample is as follows, the prepared sample is fixed on a horizontal carrying platform by a double sided adhesive tape resistant to high temperature plasma impact, one surface of a base material to be sprayed faces upwards, and the plasma spray gun is used for rotary spraying, so that the required sample is finally prepared.
As shown in table 1, three levels of the powder feeding argon gas A1, the powder feeding amount A2, the current A3, the main argon gas A4, the hydrogen gas A5, the spraying interval A6, and the turntable rotation speed A7 are all noted within the supporting range of the test equipment used in the present embodiment, as for the powder feeding amount A2, the three levels are 20g/min,25g/min, and 30g/min, respectively, which are within the supporting range of the feeding component of the plasma torch equipment.
Step S2, determining an orthogonal test table and determining a test scheme, wherein the test scheme comprises test factors and combination of factor levels, and is expressed asWhere k=1, 2,..7l=1, 2,3, indicating that Ak represents the experimental factor at level L;
for example, the orthogonal experiment table may be designed as follows:
TABLE 1
Step S3, testing according to the orthogonal test table, and measuring the porosity C1, the bonding strength C2, the hardness C3 and the dielectric constant C4 of the coating;
step S4, calculating a single factor contribution rate of powder feeding argon A1, powder feeding quantity A2, current A3, main argon A4, hydrogen A5, spraying interval A6 and rotating disc rotating speed A7 to porosity C1, bonding strength C2, hardness C3 and dielectric constant C4;
step S5, determining a comprehensive contribution rate according to the single factor contribution rate, and determining test factors corresponding to the comprehensive contribution rate exceeding a decision threshold and corresponding factor levels of the comprehensive contribution rate exceeding the decision threshold as test parameter values of the first-stage test when the comprehensive contribution rate exceeds the decision threshold of a single test index, wherein the test parameter values are n items;
s6, determining default test factors of seven test factors represented by A1-A7 in test parameter values tested in the first stage, determining default test indexes of four test indexes represented by C1-C4 in single test indexes with up-to-standard comprehensive contribution rates, and determining (7-n) default test factors;
step S7, determining test factors, factor levels and test indexes of a plasma spraying second stage test, wherein the test factors comprise seven test factors represented by A1-A7, the test factors comprise (7-n) default test factors and test parameter values of the first stage test of which the values are determined in the first stage test, the test indexes also comprise etching rate C0, the factor levels are 3 levels selected from (7-n) test factors represented by (7-n) default test factors in the range supported by corresponding test equipment, and n parameter combinations are randomly selected, and the test parameter values of the test factors in the parameter combinations are different from the test parameter values of the first stage test which are determined;
the method for testing the etching rate comprises the steps of sticking high-temperature resistant glue to the periphery of a sample, forming an etching area and an unetched area on the surface of the sample, placing the sample into a plasma etching machine for etching, and introducing gas Ar/O 2 /CF 4 (50:5:45), etching time is 10h. After etching, placing the sample in alcohol for cleaning, and then detecting the height difference at the boundary between the etched area and the unetched area by a step instrument to obtain etching depth, so as to calculate the etching rate. Therefore, when the etching rate test is carried out, the required test time is very long, the time for obtaining the production process parameters can be greatly shortened by reducing the test times of the etching rate as much as possible, and meanwhile, the loss of the etching rate test to the inner cavity of the ion etching machine can be reduced.
Step S8, determining the engravingNumerical relationship model between etching rate C0 and seven test factors represented by A1-A7Obtaining m by linear fitting k A value of (k=1, 2, …, 7);
step S9, removing the n test parameter values of the determined first stage test, comprehensively sequencing the rest (7-n) test factors to obtain the optimal factor level of each of the rest (7-n) test factors, and determining the theoretical optimal process parameter level P1-P7 of the test factors by combining the test parameter values of the first stage test;
step S10, determining an optimal process parameter interval corresponding to the optimal process parameter level of each test factor according to the step S9;
step S11, uniformly sampling in the optimal process parameter interval corresponding to the optimal process parameter level of each factor, selecting w sampling points, and generating all experimental combinations determined by the optimal process parameters, wherein the experimental combinations comprise w 7 A combination of items;
step S12, for the w 7 Obtaining a value of a predicted etching rate by using the numerical relation model f (C0) determined in the step S9, and measuring the porosity C1, the bonding strength C2, the hardness C3 and the dielectric constant C4 of the coating;
step S13, for w 7 And comprehensively sequencing the term combinations, determining the top-ranked X term parameter combinations, measuring the etching rate C0 of the X term parameter combination samples, and determining the parameter combinations of the optimal samples as final plasma spraying parameters.
In an embodiment, the calculating method of the single factor contribution rate in the step S4 is as follows:
calculate eachCorresponding individual contribution->Wherein l=1 corresponds to the lowest factor level and l=3 corresponds to the highest factor levelThe factor level corresponding to l=2 is located in the middle of the two;
for the followingThe Cd-th measurement mean of (2) is expressed as +.>Wherein d=1, 2,3,4, the measurement mean is the mean of all cds with Ak at factor level L;
for the case of l=1,the single contribution rate of (2) is calculated as follows:
for the case of l=2,the single contribution rate of (2) is calculated as follows:
for the purpose of l=3,the single contribution rate of (2) is calculated as follows:
in the step S5, a comprehensive contribution rate is determined according to the single factor contribution rate, which specifically includes: determination of
wherein Ctropt (T Ak ) Is thatThe optimal item in (2) is recorded as the Ctr corresponding factor level opt (T Ak ) Is added to the information.
For any Cd (d=1, 2,3, 4), ctr is determined opt (T Ak ) (k=1, 2,..7), and determining the optimal term combination [ Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj )]。
wherein ,Ctropt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Is Ctr opt (T Ak ) (k=1, 2,..7) the same absolute value as the optimization target direction, and recording the single factor contribution ranking order; calculating the comprehensive contribution rate ctr_all opt (Cd)=Ctr opt ′(T Ah )+Ctr opt ′(T Ai )+Ctr opt ′(T Aj )。
When Ctr opt ′(T Ah ),Ctr opt ′(T Ai ) Or Ctr opt ′(T Aj ) C1 is Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Take a negative value.
Ctr for C2-C4 opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Is the original value of (2).
In one embodiment, ctr opt (T Ak ) Is thatThe optimal term in (a) is->Or minimum value of (1), wherein:
the optimal term of the porosity C1 corresponds to the minimum term;
the optimal term of the bonding strength C2 corresponds to the maximum value term;
the optimal term of the hardness C3 corresponds to the maximum value term;
the optimum term for the dielectric constant C4 corresponds to the maximum term.
Wherein due to Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) The optimal terms are selected, so that the changing directions of the three terms are generally the same as the optimizing targets, and in addition, the etching rate is smaller and better, and the fact that C0-C1 corresponds to a negative value and C2-C4 corresponds to a positive value can be understood.
In one embodiment, when the integrated contribution rate exceeds the decision threshold of the single test index, determining the test factor corresponding to the integrated contribution rate exceeding the decision threshold and the corresponding factor level as the test parameter value of the first stage test includes:
when the comprehensive contribution rate ctr_all opt (Cd)≥Threshold deter At the time, ctr_all is determined opt (Cd) corresponding Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr op t(T Aj ) The factor level as the additional information is taken as the factor level of the corresponding test factor.
In one embodiment, when there are different integrated contribution rates ctr_all opt (Cd) is greater than the decision threshold, but when there is a conflict in the factor levels of the determined test factors, determining the test parameter values for the first stage test according to the following rules:
step S51, when the determined factor levels of the test factors have conflicts, judging the Ctr corresponding to each factor level opt The single factor contribution rank of the value in the optimal item combination, and the factor level of the top rank is determined as the test parameter value of the test factor tested in the first stage;
step S52, when the ranking of the two is the same, determining the Ctr opt The factor level corresponding to the term with the greatest absolute value of the value is determined as the test parameter value for the test factor tested in the first stage.
In an embodiment, in the step S9, the remaining (7-n) test factors are comprehensively ranked to obtain an optimal factor level of each of the remaining (7-n) test factors, and the theoretical optimal process parameter levels P1-P7 of the test factors are determined by combining the test parameter values tested in the first stage, including:
for each of the remaining (7-n) test factors, calculating the comprehensive change rate of the test index for C0-C4 under each factor level, and when the comprehensive change rate is the optimization result, determining the factor level corresponding to the optimization result as the optimal factor level of the test factor until the optimal factor level of each of the remaining (7-n) test factors is determined, and determining the theoretical optimal process parameter level P1-P7 of the test factor in combination with the test parameter value tested in the first stage.
In one embodiment, the integrated change rate is calculated by:
for each test factor of the remaining (7-n) items, each item is calculatedThe single contribution rate of the corresponding test index +.>d=0, 1,2,3,4, calculating the term +.>Corresponding comprehensive rate of change->
wherein ,the single contribution rate of the test index Cd is determined under the condition that the test factor Ak is at the factor level L;
the optimal factor level corresponding to Ak is determined as follows:
the max () function indicates a maximum function;
the optimal factor level of the remaining (7-n) items is combined with the test parameter values of the first stage test to determine theoretical optimal process parameter levels P1-P7 of the factor level of the test factor.
In an embodiment, in the step S10, an optimal process parameter interval corresponding to the optimal process parameter level of each test factor is determined according to the step S9, and specifically includes:
the optimal process parameter interval is 5% of the supporting range of the floating test equipment above and below the optimal process parameter level P1-P7 of each test factor, namely [ Pk-R ] k *5%,Pk+R k *5%](k=1, 2,..7), wherein R k And (5) supporting a test total range for the test equipment corresponding to the kth test factor.
In one embodiment, step S13, for w 7 Comprehensively sequencing the term combinations, determining X term parameter combinations with top ranking, measuring the etching rate C0 of the X term parameter combination samples, and determining the parameter combination of the optimal sample as a final plasma spraying parameter, wherein the method specifically comprises the following steps:
step s13_1, calculate w 7 Comprehensive ordering of item combinations:
for each combination of test factors Ak and the sampled value of the corresponding sampled point wCalculate each itemThe single contribution rate of the corresponding test index Cd +.>d=0, 1,2,3,4, calculating the term +.>Corresponding estimated integrated change rate->
wherein ,d=1, 2,3,4 is the single contribution determined from the measurement of C1-C4,/v>d=0 is a single contribution rate determined by obtaining a value of the predicted etching rate using the numerical relation model f (C0) determined in step S9;
step s13_2, determiningThe top X parameter combination samples are used for carrying out etching rate C0 measurement to obtain a measured value VL of C0-C4 of each sample in the X parameter combination samples C0 -VL C4 An optimized evaluation value TVL for each sample is calculated, tvl=vl C4 +VL C3 +VL C2 -VL C1 -VL C0
And step S13-3, combining parameters of the sample with the maximum TVL value as final plasma spraying parameters.
In a certain embodiment, a non-volatile computer storage medium is provided, which stores computer executable instructions that perform the method steps described in the above embodiments.
Compared with the prior art, the method provided by the invention has the advantages that the optimal parameters are found in the plasma spraying parameter data test, the corrosion influence degree of the plasma etching process is reduced by reducing the test times of the etching rate, the spraying effect is better, the efficiency is higher, and the spraying quality is higher. The test quality can be ensured, important influencing factors are avoided, the test time can be saved, meanwhile, the short plate of the traditional orthogonal experiment is made up, the optimal parameters of the orthogonal experiment are limited to the optimal combination of factor levels, and the method is a section with a larger range and can not really find the optimal parameters of equipment.
It should be noted that the computer readable medium described in the present disclosure may be a computer readable signal medium or a computer readable storage medium, or any combination of the two. The computer readable storage medium can be, for example, but not limited to, an electronic, magnetic, optical, electromagnetic, infrared, or semiconductor system, apparatus, or device, or a combination of any of the foregoing. More specific examples of the computer-readable storage medium may include, but are not limited to: an electrical connection having one or more wires, a portable computer diskette, a hard disk, a Random Access Memory (RAM), a read-only memory (ROM), an erasable programmable read-only memory (EPROM or flash memory), an optical fiber, a portable compact disc read-only memory (CD-ROM), an optical storage device, a magnetic storage device, or any suitable combination of the foregoing. In the context of this disclosure, a computer-readable storage medium may be any tangible medium that can contain, or store a program for use by or in connection with an instruction execution system, apparatus, or device. In the present disclosure, however, the computer-readable signal medium may include a data signal propagated in baseband or as part of a carrier wave, with the computer-readable program code embodied therein. Such a propagated data signal may take any of a variety of forms, including, but not limited to, electro-magnetic, optical, or any suitable combination of the foregoing. A computer readable signal medium may also be any computer readable medium that is not a computer readable storage medium and that can communicate, propagate, or transport a program for use by or in connection with an instruction execution system, apparatus, or device. Program code embodied on a computer readable medium may be transmitted using any appropriate medium, including but not limited to: electrical wires, fiber optic cables, RF (radio frequency), and the like, or any suitable combination of the foregoing.
The computer readable medium may be contained in the electronic device; or may exist alone without being incorporated into the electronic device.
Computer program code for carrying out operations of the present disclosure may be written in one or more programming languages, including an object oriented programming language such as Java, smalltalk, C ++ and conventional procedural programming languages, such as the "C" programming language or similar programming languages. The program code may execute entirely on the user's computer, partly on the user's computer, as a stand-alone software package, partly on the user's computer and partly on a remote computer or entirely on the remote computer or server. In the case of a remote computer, the remote computer may be connected to the user's computer through any kind of network, including a Local Area Network (LAN) or a Wide Area Network (WAN), or may be connected to an external computer (for example, through the Internet using an Internet service provider).
The flowcharts and block diagrams in the figures illustrate the architecture, functionality, and operation of possible implementations of systems, methods and computer program products according to various embodiments of the present disclosure. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of code, which comprises one or more executable instructions for implementing the specified logical function(s). It should also be noted that, in some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems which perform the specified functions or acts, or combinations of special purpose hardware and computer instructions.
The units involved in the embodiments of the present disclosure may be implemented by means of software, or may be implemented by means of hardware. Wherein the names of the units do not constitute a limitation of the units themselves in some cases.
The foregoing description of the preferred embodiments of the present invention has been presented for purposes of clarity and understanding, and is not intended to limit the invention to the particular embodiments disclosed, but is intended to cover all modifications, alternatives, and improvements within the spirit and scope of the invention as outlined by the appended claims.

Claims (10)

1. A plasma spraying parameter determining method comprises the following steps:
step S1, determining test factors, factor levels and test indexes of a plasma spraying first stage test, wherein the test factors comprise powder feeding argon A1, powder feeding quantity A2, current A3, main argon A4, hydrogen A5, spraying interval A6 and rotating disc rotating speed A7, the test indexes comprise porosity C1, bonding strength C2, hardness C3 and dielectric constant C4 of a coating, and the factor levels are that 3 levels are selected from seven test factors represented by the A1-A7 in a range supported by test equipment;
step S2, determining an orthogonal test table and a test scheme, wherein the test scheme comprises test factors and combination of factor levels, and is expressed asWherein k=1, 2, …,7, l=1, 2,3, indicating that Ak represents the experimental factor takes on a value at level L;
step S3, testing according to the orthogonal test table, and measuring the porosity C1, the bonding strength C2, the hardness C3 and the dielectric constant C4 of the coating;
s4, calculating single-factor contribution rates of powder feeding argon A1, powder feeding quantity A2, current A3, main argon A4, hydrogen A5, spraying interval A6 and rotating disc rotating speed A7 to porosity C1, bonding strength C2, hardness C3 and dielectric constant C4;
step S5, determining a comprehensive contribution rate according to the single factor contribution rate, and determining test factors corresponding to the comprehensive contribution rate exceeding a decision threshold and corresponding factor levels of the comprehensive contribution rate exceeding the decision threshold as test parameter values of the first-stage test when the comprehensive contribution rate exceeds the decision threshold of a single test index, wherein the test parameter values are n items;
s6, determining default test factors of seven test factors represented by A1-A7 in test parameter values tested in the first stage, determining default test indexes of four test indexes represented by C1-C4 in single test indexes with up-to-standard comprehensive contribution rates, and determining (7-n) default test factors;
step S7, determining test factors, factor levels and test indexes of a plasma spraying second stage test, wherein the test factors comprise seven test factors represented by A1-A7, the test factors comprise (7-n) default test factors and test parameter values of the first stage test of which the values are determined in the first stage test, the test indexes also comprise etching rate C0, the factor levels are 3 levels selected from (7-n) test factors represented by (7-n) default test factors in the range supported by corresponding test equipment, and n parameter combinations are randomly selected, and the test parameter values of the test factors in the parameter combinations are different from the test parameter values of the first stage test which are determined;
step S8, determining a numerical relation model between the etching rate C0 and seven test factors represented by A1-A7Obtaining m by linear fitting k Wherein k=1, 2, …,7;
step S9, removing the n test parameter values of the determined first stage test, comprehensively sequencing the rest (7-n) test factors to obtain the optimal factor level of each of the rest (7-n) test factors, and determining the theoretical optimal process parameter level P1-P7 of the test factors by combining the test parameter values of the first stage test;
step S10, determining an optimal process parameter interval corresponding to the optimal process parameter level of each test factor according to the step S9;
step S11, at each factorUniformly sampling in an optimal process parameter interval corresponding to the optimal process parameter level, selecting w sampling points, and generating all experimental combinations determined by the optimal process parameters, wherein the experimental combinations comprise w 7 A combination of items;
step S12, for the w 7 Obtaining a value of a predicted etching rate using the numerical relation model f (C0) determined in step S9, and measuring the porosity C1, the bonding strength C2, the hardness C3, and the dielectric constant C4 of the coating;
step S13, for w 7 And comprehensively sequencing the term combinations, determining the top-ranked X term parameter combinations, measuring the etching rate C0 of the X term parameter combination samples, and determining the parameter combinations of the optimal samples as final plasma spraying parameters.
2. The plasma spraying parameter determining method according to claim 1, wherein the calculating method of the single factor contribution rate in step S4 is as follows:
calculate eachCorresponding individual contribution->Wherein the factor level corresponding to l=1 is lowest, the factor level corresponding to l=3 is highest, and the factor level corresponding to l=2 is located in the middle of the two;
for the followingThe Cd-th measurement mean of (2) is expressed as +.>Wherein d=1, 2,3,4, the measurement mean is the mean of all cds with Ak at factor level L;
for the case of l=1,the single contribution rate of (2) is calculated as follows:
for the case of l=2,the single contribution rate of (2) is calculated as follows:
for the purpose of l=3,the single contribution rate of (2) is calculated as follows:
3. the plasma spraying parameter determining method according to claim 1, wherein the determining of the comprehensive contribution rate in step S5 according to the single factor contribution rate is specifically: determination of wherein Ctropt (T Ak ) Is->The optimal item in (2) is recorded as the Ctr corresponding factor level opt (T Ak ) Is added to the information;
for any Cd, where d=1, 2,3,4, ctr is determined opt (T Ak ) Where k=1, 2, …,7, and determining the optimal term combination [ Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj )]Wherein, ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Is Ctr opt (T Ak ) The three items with the maximum absolute value values, which are the same as the direction of the optimization target, are recorded, and the ranking order of the contribution of the single factors is recorded;
calculating the comprehensive contribution rate:
Ctr_ALL opt (Cd)=Ctr opt ′(T Ah )+Ctr opt ′(T Ai )+Ctr opt ′(T Aj ),
when Ctr opt ′(TAh),Ctr opt ′(T Ai ) Or Ctr opt ′(T Aj ) C1 is Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Taking a negative value;
ctr for C2-C4 opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) Is the original value of (2).
4. The plasma spray parameter determination method as recited in claim 3, wherein Ctr opt (T Ak ) Is thatThe optimal term in (a) isOr minimum value of (1), wherein:
the optimal term of the porosity C1 corresponds to the minimum term; the optimal term of the bonding strength C2 corresponds to the maximum value term; the optimal term of the hardness C3 corresponds to the maximum value term; the optimum term for the dielectric constant C4 corresponds to the maximum term.
5. The plasma spray parameter determination method according to claim 1, wherein when the integrated contribution rate exceeds a decision threshold of a single test index, determining a test factor corresponding to the integrated contribution rate exceeding the decision threshold and a corresponding factor level as a test parameter value of the first stage test, comprises:
when the comprehensive contribution rate ctr_all opt (Cd)≥Threshold deter At the time, ctr_all is determined opt (Cd) corresponding Ctr opt (T Ah ),Ctr opt (T Ai ),Ctr opt (T Aj ) The factor level as the additional information is taken as the factor level of the corresponding test factor.
6. The method of claim 5, wherein when there are different integrated contribution rates ctr_all opt (Cd) is greater than the decision threshold, but when there is a conflict in the factor levels of the determined test factors, determining the test parameter values for the first stage test according to the following rules:
step S51, when the determined factor levels of the test factors have conflicts, judging the Ctr corresponding to each factor level opt The single factor contribution rank of the value in the optimal item combination, and the factor level of the top rank is determined as the test parameter value of the test factor tested in the first stage;
step S52, when the ranking of the two is the same, determining the Ctr opt The factor level corresponding to the term with the greatest absolute value of the value is determined as the test parameter value for the test factor tested in the first stage.
7. The plasma spraying parameter determining method as claimed in any one of claims 1 to 2, wherein in the step S9, the remaining (7-n) test factors are comprehensively sorted to obtain an optimal factor level of each of the remaining (7-n) test factors, and determining the theoretical optimal process parameter level P1-P7 of the test factors in combination with the test parameter values of the first stage test comprises:
for each of the remaining (7-n) test factors, calculating the comprehensive change rate of the test index for C0-C4 under each factor level, and when the comprehensive change rate is the optimization result, determining the factor level corresponding to the optimization result as the optimal factor level of the test factor until the optimal factor level of each of the remaining (7-n) test factors is determined, and determining the theoretical optimal process parameter level P1-P7 of the test factor in combination with the test parameter value tested in the first stage.
8. The plasma spray parameter determination method as claimed in claim 7, wherein the comprehensive change rate is calculated by:
for each test factor of the remaining (7-n) items, each item is calculatedThe single contribution rate of the corresponding test index +.>Calculate the item +.>Corresponding comprehensive rate of change->
wherein ,the single contribution rate of the test index Cd is determined under the condition that the test factor Ak is at the factor level L;
the optimal factor level corresponding to Ak is determined as follows:
the max () function indicates a maximum function;
the optimal factor level of the remaining (7-n) items is combined with the test parameter values of the first stage test to determine theoretical optimal process parameter levels P1-P7 of the factor level of the test factor.
9. The plasma spraying parameter determining method according to claim 1, wherein in the step S10, an optimal process parameter interval corresponding to the optimal process parameter level of each test factor is determined according to the step S9, specifically:
the optimal process parameter interval is 5% of the supporting range of the floating test equipment above and below the optimal process parameter level P1-P7 of each test factor, namely [ Pk-R ] k *5%,Pk+R k *5%]Where k=1, 2, …,7, where R k And (5) supporting a test total range for the test equipment corresponding to the kth test factor.
10. The method of determining plasma spraying parameters according to claim 1, wherein in step S13, w 7 Comprehensively sequencing the term combinations, determining X term parameter combinations with top ranking, measuring the etching rate C0 of the X term parameter combination samples, and determining the parameter combination of the optimal sample as a final plasma spraying parameter, wherein the method specifically comprises the following steps:
step s13_1, calculate w 7 Comprehensive ordering of item combinations:
for each combination of test factors Ak and the sampled value of the corresponding sampled point wCalculate each item +.>The single contribution rate of the corresponding test index Cd +.>Calculate the item +.>Corresponding estimated integrated change rate->
wherein ,for a single contribution rate determined from the C1-C4 measurements,obtaining a single contribution rate determined for a value of the predicted etching rate using the numerical relation model f (C0) determined in step S9;
step s13_2, determiningThe top X parameter combination samples are used for carrying out etching rate C0 measurement to obtain a measured value VL of C0-C4 of each sample in the X parameter combination samples C0 -VL C4 Calculating an optimized evaluation value TVL of each sample;
TVL=VL C4 +VL C3 +VL C2 -VL C1 -VL C0
and step S13-3, combining parameters of the sample with the maximum TVL value as final plasma spraying parameters.
CN202211503716.4A 2022-11-28 2022-11-28 Plasma spraying parameter determination method Active CN115828574B (en)

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