CN105881694B - A kind of screening technique of the rapid condensation proportioning of rock-like materials - Google Patents
A kind of screening technique of the rapid condensation proportioning of rock-like materials Download PDFInfo
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- CN105881694B CN105881694B CN201610220412.5A CN201610220412A CN105881694B CN 105881694 B CN105881694 B CN 105881694B CN 201610220412 A CN201610220412 A CN 201610220412A CN 105881694 B CN105881694 B CN 105881694B
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- 239000000463 material Substances 0.000 title claims abstract description 186
- 238000000034 method Methods 0.000 title claims abstract description 65
- 238000009833 condensation Methods 0.000 title claims abstract description 11
- 230000005494 condensation Effects 0.000 title claims abstract description 11
- 238000012216 screening Methods 0.000 title claims abstract description 8
- 238000010146 3D printing Methods 0.000 claims abstract description 41
- 239000004568 cement Substances 0.000 claims abstract description 39
- 230000004044 response Effects 0.000 claims abstract description 28
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- 238000005211 surface analysis Methods 0.000 claims abstract description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- 239000010440 gypsum Substances 0.000 claims description 43
- 229910052602 gypsum Inorganic materials 0.000 claims description 43
- 238000002156 mixing Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 14
- 238000013461 design Methods 0.000 claims description 13
- 238000009826 distribution Methods 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 10
- 238000007639 printing Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- 238000012887 quadratic function Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 4
- 238000013507 mapping Methods 0.000 claims description 3
- 239000011435 rock Substances 0.000 claims description 3
- 238000013459 approach Methods 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims 1
- 238000012549 training Methods 0.000 claims 1
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 15
- 230000008859 change Effects 0.000 description 13
- 238000011161 development Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
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- 230000003746 surface roughness Effects 0.000 description 3
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- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012913 prioritisation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940036811 bone meal Drugs 0.000 description 1
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- 238000004364 calculation method Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y50/00—Data acquisition or data processing for additive manufacturing
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Mechanical Engineering (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides the screening technique that a kind of rapid condensation of rock-like materials matches.The present invention is from abundant printed material species and the angle for reducing cost, for application prospect of the material in 3D printing technique, several main materials and its specificity analysis are given first, and requirement of the 3D printing technique to printed material is studied, selection meets the material of 3D printing technique requirement, such as land plaster and accelerated cement from material；On this basis, combining response Surface Analysis method is compared analysis to presetting period of the selected material under different ratio and final setting time, finally selects the gradation of drop-out colour for best suiting requirement.
Description
Technical field
The present invention relates to the screening technique that a kind of rapid condensation of rock-like materials matches, and belongs to material preparation technology neck
Domain.
Background technology
The unification of 3D printing material category and highization of cost are to govern the master of 3D printing technique popularization and development
Want reason.
Present well known 3D printing technique is to come across mid-term the 1990s earliest, but due to making at that time
Costly, technology is also relatively less ripe for cost lattice, so early stage 3D printing technique is not promoted widely.And such as
The present, 3D technology have passed through the development of more than 20 years, and technology is more ripe, control is also more accurate, and manufacturing cost also has
Reduced.But the unification of printed material and highization are still to restrict a major reason of 3D printing technique development.
At present according to different printing devices, printed material mainly include engineering plastics, photosensitive resin, rubber type of material,
Metal material and ceramic material etc., in addition, the food such as coloured plaster material, artificial bone meal, cell biological raw material and granulated sugar
Product material is also applied in 3D printing field.These raw material used in 3D printing be all specific to 3D printing equipment and
Technique and research and develop, it is otherwise varied with common plastics, gypsum, resin etc., its form typically have powdered, thread, lamellar,
It is liquid etc..Generally, according to the type of printing device and the difference of operating condition, used powdered 3D printing material it is straight
Footpath is 1-100 μm.
In recent years, 3D printing technique develops year by year, and the field applied is also more and more extensive, but the supply of printed material
Allow of no optimist.The 3D printing material in China is primarily present some following problem at present：
1st, material property does not reach requirement, influences the popularization of 3D printing；
2nd, material category can be used on the low side, it is difficult to meet 3D printing demand；
3rd, material cost is higher, limits application field；
4th, 3D printing material in China part relies on import, limits commercial application.
Printed material is the basis of 3D printing development, and 3D printing technique and the ripe of equipment can also promote holding for material property
Hair and perfect, expansion description of materials and application.At present, China part 3D printing technique and equipment are first intake in the world
It is flat, but larger gap compared with advanced country also be present in material development and application aspect, therefore break material and 3D printing is sent out
The restriction of exhibition is very crucial.
The content of the invention
To reach above-mentioned purpose, the invention provides the screening technique that a kind of rapid condensation of rock-like materials matches, and leads to
The combination of materials of suitable 3D printing can be selected by crossing this method, and combining response face method was analyzed its setting time, so as to select
Go out optimal printed material.
To reach above-mentioned purpose, the invention provides a kind of rock-like materials rapid condensation match screening technique, its
Comprise the following steps：
(1) at least two materials are selected as detected materials according to general requirement of the 3D printing technique to material；
(2) combining response face method determines different experiment proportionings, i.e. ratio between detected materials and water, establishes response surface
Analysis model, and detected materials and water are mixed to get mixing material according to different experiment proportionings, it is real that 3D printing is carried out respectively
Test, obtain presetting period, the measured value of final setting time of the mixing material of different experiments proportioning；Using orthogonal experimental design method pair
It is grouped, can be selected according to the situation of detected materials, generally more than 10 groups in experiment proportioning；Pass through orthogonal experiment
Design method is grouped, and grouping experiment finishes, and can obtain the model between mixting ratio factor using response phase method, passes through model point
Analysis can obtain obtaining optimum proportioning；
With response surface design analyze method be fitted, obtain concentration of the detected materials in the mixing material with just
Solidifying time, the functional relation of final setting time, and then obtain presetting period, the predicted value of final setting time；
Establish the normal distribution of the presetting period of mixture, the experiment value of final setting time and predicted value that different experiments match
Figure, experimental analysis variogram, residual error and prognostic chart, prediction and actual figure, prediction and runtime value figure and the quality of detected materials
Contour map, three-dimensional response surface design figure between the volume of water；
Pass through experimental analysis variogram, fitting quadratic regression equation, residual plot, predicted value figure, contour map, three-dimensional response
Surface chart, optimize the value of the quality of detected materials and the volume of water, make its response in corresponding mapping range and defeated
Go out the response of minimum；Specific analysis may be referred to conventional analysis and carry out, such as conventional residual analysis method etc.；
Analyze the normal distribution, experimental analysis variogram, residual error and prognostic chart, prediction and actual figure, prediction and fortune
Row value figure, and by experiment obtain the presetting period, final setting time experiment value, to the experiment value carry out response surface analysis, obtain
To regression model, and presetting period, the theoretical value of final setting time are calculated, and obtain presetting period, the predicted value of final setting time
Mutual functional relation between the quality of quality with detected materials, the functional relation between the volume of water and detected materials；
(3) according to center combination design, with reference to the result obtained in step (2), the fit equation pair of quadratic function is utilized
Presetting period, final setting time are fitted, and the proportion optimizing scheme of detected materials and water and corresponding is obtained according to fitting result
Presetting period, final setting time, desired value；
(4) 3D printing experiment is carried out again according to the detected materials of the quality such as proportion optimizing scheme, selection and water, obtain excellent
Change presetting period, the experiment value of final setting time of mix proportion scheme, and by experiment value compared with theoretical value, obtain relative miss
Difference, judge whether fitting is reasonable：If rationally, the selection wherein presetting period is most short, minimum it is expected, final setting time rational one assembles
Than the mixing material gone out with the proportional arrangement is the material of rock-like materials 3D printing；
If unreasonable, repeat step (3), until obtaining rational fitting result.
In the above-mentioned methods, it is preferable that in step (1), 3D printing technique requires to include to the general of material：Be advantageous to
Fast, accurately process prototype parts；Rapid shaping product should approach final requirement, meet to intensity, rigidity, humidity
Property, the requirement of thermal stability；Be advantageous to follow-up handling process., can be by people in the art when selecting detected materials
Member is carried out using principal element in a conventional manner according to actual conditions.
In the above-mentioned methods, it is preferable that normal distribution is the studentized residuals of detected materials and the pass of mass percent
It is curve, the studentized residuals are abscissa, and the mass percent is ordinate.
In the above-mentioned methods, it is preferable that residual error is the predicted value of detected materials and the relation of studentized residuals with prognostic chart
Curve, the residual error are ordinate, and the predicted value is abscissa.
In the above-mentioned methods, it is preferable that prediction and the relation curve that actual figure is the predicted value and actual value, wherein,
The predicted value is ordinate, and the actual value is abscissa.
In the above-mentioned methods, it is preferable that prediction is that the studentized residuals and the relation of operation sequence number are bent with runtime value figure
Line, the studentized residuals are ordinate, the operation serial number abscissa.
In the above-mentioned methods, it is preferable that the 3D printing experiment in step (2) and step (4) follows the steps below：Press
According to the facts test proportioning and weigh various detected materials and water；Detected materials are mixed with water, obtain mixing material；Mixing material is inserted
The extrusion device of 3D printer, stirred when inserting, prevent rocks class condensation of materials；The extrusion device of mixing material will be installed
It is fixed on 3D printer, starts the reducing motor of printing, mixing material is squeezed out from extrusion device, and on chassis
Heated, accelerate the rate of set of rock-like materials, be allowed to rapid shaping, complete experiment, in forming process, collection
The extruded velocity of mixing material, the heating-up temperature on chassis, presetting period, final setting time.
Present invention also offers a kind of rock-like materials 3D printing material, and it is prepared by the proportioning obtained according to the method described above
, the material includes gypsum, cement, water, and the ratio of three is 9.35g：5g：6.12mL.
The present invention is from abundant printed material species and the angle for reducing cost, for material in 3D printing technique
Application prospect, several main materials and its specificity analysis are given first, and to requirement of the 3D printing technique to printed material
Studied, the material for meeting 3D printing technique requirement, such as land plaster and accelerated cement are selected from material；It is basic herein
On, combining response Surface Analysis method is compared point to presetting period of the selected material under different ratio and final setting time
Analysis, finally selects the gradation of drop-out colour for best suiting requirement.
Brief description of the drawings
Fig. 1 is the residual error in presetting period and the graph of a relation of percentage of materials A.
Fig. 2 is the residual error in presetting period and the graph of a relation of predicted value of materials A.
Fig. 3 is the predicted value in presetting period and the graph of a relation of actual value of materials A.
Fig. 4 is the predicted value in presetting period and the graph of a relation of runtime value of materials A.
Fig. 5 is the actual value in gypsum presetting period and the contrast line chart of predicted value.
Fig. 6 A, Fig. 6 B, Fig. 6 C are respectively the contour map between material B and water.
Fig. 7 A, Fig. 7 B, Fig. 7 C are respectively the contour map between materials A and water.
Fig. 8 A, Fig. 8 B, Fig. 8 C are respectively the three-dimensional response surface design figure between materials A and material B.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment
A kind of screening technique of the rapid condensation proportioning of rock-like materials is present embodiments provided, it comprises the following steps：
First, experiment material is chosen
Select material according to general requirement of the 3D printing technique to material, the performance requirement of printed material meet it is following some
：
1st, setting strength it is higher (>=42.5MPa) --- avoid collapsing when stacking；
2nd, the rate of set moderate (presetting period<=30s) --- it can not combine between layers soon very much, it is too slow to stack at present
Layer does not cool down also, and the getting off to produce of upper strata collapses；
3rd, smokeless odorlessness --- harm is not produced to environment and human body；
4th, material good moldability --- to ensure the size of printout and precision.
The present embodiment selection with some strength, the gypsum of hardness and good stability and rapid hardening, corrosion-resistant, high temperature resistant and
The higher cement of intensity is as detected materials, and the essential characteristic and the scope of application of selected land plaster and cement are as shown in table 1, table 2.
Table 1
Table 2
2nd, experimental design and operation
Combining response face method determines different experiment proportionings, i.e. ratio between land plaster, cement, water：
Gypsum 5-15g, cement 5-15g, water 6-12mL are chosen, three kinds of materials are entered according to different proportion in the range of this
Row mixing, establishes response surface analysis model, obtains 17 groups of different mix proportion schemes, as shown in table 3.
3 17 groups of mix proportion schemes of table
Tested in strict accordance with the step of sampling, stirring, filler, printing and cleaning apparatus, due to manufacturing process more
Complexity, influence factor is also relatively more, and any operational error will all produce large effect to result of the test, therefore, each
The concrete operations of step are as follows：
(1) sample
Matched according to the experiment given by table 3, electronic scale weighs various materials：Gypsum, cement, water.
(2) mix thoroughly
Gypsum, cement are poured into agitator successively, then pour into water while stirring, until stirring, is mixed
Material.
(3) filler
The mixing material to stir is inserted in the extrusion device of 3D printer, stirred when being put into, prevent rocks
Class condensation of materials.
(4) print
Charged extrusion device is fixed on 3D printer, starts the reducing motor of printing, material is filled from extrusion
Squeeze out in putting, and heated on chassis, accelerate the rate of set of rock-like materials, be allowed to rapid shaping.
In forming process, the parameter such as the extruded velocity of capturing material, the heating-up temperature on chassis.
(5) cleaning apparatus
After the completion of printing, device used in experiment is cleared up rapidly, conserved, prevents rock-like materials from condensing in utensil
On, cause unnecessary damage.
3rd, test result analysis
Because presetting period of the material under different ratio, final setting time are difficult to be expressed with a definite equation, but pass through
Substantial amounts of experiment is crossed, is obtained under a series of various concentrations (17 groups of different ratio schemes of gypsum, cement, water i.e. shown in table 3)
Setting time (as shown in table 4), with response surface design analyze method, these data are fitted, approximately obtain material
Expect concentration and the functional relation of setting time.
Setting time under the different materials concentration of table 4
Input quantity in experiment has three, the i.e. quality of gypsum, the quality of cement, the volume of water, using least square method
Analysis is fitted to it, takes testing site m=17 (according to Responds Surface Methodology, to choose 17 groups shown in table 3 suitable matching somebody with somebody and suppose
Case, therefore select m=17, i.e., be fitted to 17 groups of data), undetermined coefficient γi=3 (corresponding to three input quantities), therefore function
Form is the quadratic form containing intercrossing, as shown in formula 1.1：
Wherein：a0For constant term undetermined coefficient, aiFor first order undetermined coefficient, aijFor quadratic term undetermined coefficient；
In order to be fitted conveniently, approximate quadratic function is converted into the linear forms for increasing dimension by substitution of variable, coefficient becomes
The formula of changing is：
α0=γ0, α1=γ1..., αk=γk, αk+1=γ11... αn-1=γkk
Therefore linear regression function model is expressed as：
17 testing sites are brought into formula (1.2), obtain the estimated value (i.e. predicted value) of testing site：
Matrix form is：
In formulaIt is vectorial for undetermined coefficient,
To test dot matrix,
For experiment estimate vector.
The then actual value (actual value is obtained by experiment, is the setting time under different ratio herein) of the m times
For：
Y={ y(0)..., y(m-1)}T
TakeThen e is the predicted value and n experiment the data obtained of linear model
The stochastic variable of error, wherein eiAverage be 0, variance σ.
To cause eiQuadratic sum it is minimum, then the minimum value of modus ponens 1.4：
Wherein, e is the error vector of experiment value and predicted value, and L is a median, simply a kind of expression way；Y is true
Real value (experiment value),For predicted value, x represents the quality of gypsum, the quality of cement, the volume of water, and γ is treating for fit equation
Determine coefficient.
I.e.：
(1.3) are brought into (1.5), obtained：
And：
γ=(xTx)-1xTy (1.8)
When x is square formation and nonsingular, then
γ=x-1y (1.9)
Unique γ can be obtained according to m testing site, bring formula (1.9) into formula (1.6), as L=0, that is, drawn every
The estimate of individual testing site is equal to test value.
Pass through data point distribution figure, two such as experimental analysis variogram, fitting quadratic regression equation, residual plot, predicted value figure
The contour of secondary item and three-dimensional response surface design figure etc..Optimize three factors (gypsum quality, rapid-curing cutback cement quality, the volume of water),
Make its response in corresponding mapping range and export the response of minimum.
Experiment sets input quantity as three, respectively the quality (span 5-15g) of materials A gypsum, material B cement
Quality (span 5-15g), the volume (span 6-12mL) of material C water；Output quantity two, the presetting period of mixture
t1, final setting time t2, unit is the second.
Experiment is divided into 17 groups (as shown in table 3), and it is inputted, output valve is as shown in table 5：
The experiment of table 5 input, output valve
| Test number (TN) | Materials A：Gypsum (g) | Material B：Cement (g) | Material C：Water (mL) | Presetting period (t) | Final setting time (t) |
| 1 | 10.00 | 10.00 | 9.00 | 7 | 11 |
| 2 | 5.00 | 10.00 | 12.00 | 49 | 38 |
| 3 | 10.00 | 10.00 | 9.00 | 7 | 11 |
| 4 | 15.00 | 15.00 | 9.00 | 13 | 4 |
| 5 | 5.00 | 10.00 | 6.00 | 13 | 7 |
| 6 | 15.00 | 5.00 | 9.00 | 2 | 10 |
| 7 | 10.00 | 10.00 | 9.00 | 7 | 11 |
| 8 | 5.00 | 15.00 | 9.00 | 11 | 7 |
| 9 | 15.00 | 10.00 | 12.00 | 8 | 6 |
| 10 | 10.00 | 15.00 | 12.00 | 11 | 5 |
| 11 | 10.00 | 10.00 | 9.00 | 7 | 11 |
| 12 | 10.00 | 10.00 | 9.00 | 7 | 11 |
| 13 | 5.00 | 5.00 | 9.00 | 17 | 10 |
| 14 | 10.00 | 5.00 | 12.00 | 14 | 7 |
| 15 | 10.00 | 15.00 | 6.00 | 4 | 5 |
| 16 | 15.00 | 10.00 | 6.00 | 15 | 7 |
| 17 | 10.00 | 15.00 | 6.00 | 14 | 6 |
A, material and presetting period, the relation of final setting time
By taking materials A (gypsum) as an example, to its normal distribution, residual error and prognostic chart, prediction and actual figure, prediction and operation
Value figure (gypsum of these figures in table 5, cement, the quality of water and corresponding presetting period, final setting time obtain) is divided
Analysis：
The quality of gypsum, cement and water is represented with A, B, C respectively, experiment value (is broken the material under different ratio
Print experiment, resulting presetting period, the experiment value of final setting time) regression fit is carried out, the regression model in presetting period is established, its
Expression formula is：
By the model obtain the presetting period, final setting time theoretical value, R1Represent presetting period, R2Represent final setting time；
In two above fit equation, the relevant parameter of presetting period and final setting time is as shown in table 6 and table 7.Pass through
The fianalysis tting degree of two equations can show that the fitting degree of the mathematical modeling is higher, can be used for predicting.With the presetting period
Mathematical modeling with final setting time is object function, using the mathematical modeling of the volume of the quality of gypsum, the quality of cement and water as
Constraint function, the equation of composition have the point such as multivariable, non-linear, Constrained.
The coefficient correlation of 6 presetting period of table model
| Project | Numerical value |
| Quadratic sum (sum of squares) | 479.51 |
| Square (mean square) | 159.84 |
| The free degree (DOF) | 3 |
| Standard on data deviation (Std.Dev.) | 4.56 |
| The coefficient of determination (R-Squared) | 0.9154 |
| Correct degree of fitting (Adj-R-Squared) | 0.8066 |
| Predict degree of fitting (Pred R-Squared) | -0.3537 |
| Signal to noise ratio (Adep Precision) | 12.726 |
The coefficient correlation of the final setting time model of table 7
| Project | Numerical value |
| Quadratic sum (sum of squares) | 177.97 |
| Square (mean square) | 59.32 |
| The free degree (DOF) | 3 |
| Standard on data deviation (Std.Dev.) | 5.58 |
| The coefficient of determination (R-Squared) | 0.7684 |
| Correct degree of fitting (Adj-R-Squared) | 0.4707 |
| Predict degree of fitting (Pred R-Squared) | -2.7052 |
| Signal to noise ratio (Adep Precision) | 6.859 |
(1) as shown in figure 1, using the studentized residuals of materials A (gypsum) output valve as abscissa, sat using its percentage to be vertical
Mark, its curve of output can approximately regard straight line as, so its error meets normal distribution.Frequency test result such as table 8
It is shown.
(2) when being ordinate using predicted value as abscissa, residual error, the point described is equal to 0 straight line around residual values
Upper and lower random scatter, in addition to two points, other are all distributed between (- 2,2), and without any system trends, then it is assumed that
Regression straight line and the fit solution of former observation are good, and quality and the presetting period of materials A (gypsum) have more significantly linearly
Relation.Residual error is as shown in Figure 2 with prognostic chart.
The frequency test result of table 8
| ξ | (- 1,1) | (- 1.5,1.5) | (- 2,2) |
| P | 0.41 | 0.76 | 0.88 |
| [P] | 0.68 | 0.87 | 0.95 |
(3) it is ordinate by abscissa, predicted value of the actual value of materials A (gypsum), after rejecting Null Spot, predicted value is enclosed
Upper and lower around actual value is distributed around, and approximate fits are straight line, and setting time between 2 to 17, as shown in Figure 3.
(4) be ordinate with operation serial number abscissa, studentized residuals, after rejecting irrational point, residual values without
Rule is distributed between (- 2,2), then it is assumed that the fit equation of predicted value substantially conforms to actual equations, and prediction and service chart are such as
Shown in Fig. 4.
In summary, the experiment value of materials A (gypsum) and predicted value are in the range of reasonable error, its quality and presetting period
Substantially conform to linear relationship.The result of calculation that the mass value of gypsum as shown in table 3 passes through formula (1.10) is pre- in table 9
Measured value, the experiment value for table 9 resulting by printing experiment.Experiment value and predicted value contrast are as shown in table 9, broken line such as Fig. 5
It is shown.
The presetting period experiment value of the materials A of table 9 (gypsum) and predicted value contrast table
Although actual value and the predicted value discrepancy of some, generally about in predicted value or so, you can think to intend
It is reasonable to close equation.
B, the interaction relationship between material
(1) when materials A (gypsum) takes 5g, 10g, 15g respectively in interval range, material B (cement) and material C (water)
Between influence each other as shown in Fig. 6 A, Fig. 6 B, Fig. 6 C, wherein, abscissa is the quality of cement, and ordinate is the volume of water.
From Fig. 6 A, Fig. 6 B, Fig. 6 C, when materials A (gypsum) is 5g, the volume of material C (water) is not substantially with material B
The mass change of (cement) and change, its value is centered around 8mL and fluctuated, if it is therefore contemplated that 5g gypsum is completely dissolved
Need water 8mL.When gypsum takes 10g, cement to take 6.5-9g, the volume of water increases and increased with cement quality, and linear change
Change, after cement is more than 9g, beyond soluble end, the volume of water is held essentially constant.When gypsum takes 15g, the volume of water
Increase as cement quality increases, but amplitude change is smaller.In summary, as the timing of value one of materials A (gypsum), material B
The quality of (cement) and the linear dependency relation of volume of material C (water).
With the change of materials A (gypsum) quality, the presetting period of mixture also changes therewith, and variation tendency is in secondary
Distribution.When the quality of materials A (gypsum) is smaller change it is more notable, when materials A (gypsum) quality between 7-10g time-varying
Change more slow.
(2) when material B (cement) takes 5g, 10g, 15g in interval range, between materials A (gypsum) and material C (water)
Influence each other as shown in Fig. 7 A, Fig. 7 B, Fig. 7 C, wherein, the volume that abscissa is cement quality, ordinate is water.
It can similarly obtain, when material B (cement) timing of value one, the linear phase of quality of materials A (gypsum) and material C (water)
Pass relation, and correlation is more than A and C correlation, the i.e. water solubility of gypsum better.
With the change of material B (cement) quality, the presetting period of mixture also changes therewith, and variation tendency is in secondary
Distribution, curvature are less than curvature when materials A (gypsum) changes.When material B (cement) quality becomes in 5g or so, its presetting period
Change smaller.
(3) when material C (water) takes different value in interval range, the phase between materials A (gypsum) and material B (cement)
Mutually influence as shown in Fig. 8 A, Fig. 8 B, Fig. 8 C, wherein, the quality that X-axis is the quality of gypsum, Y-axis is cement, when Z axis is pre-hardening
Between.
It is can be seen that from Fig. 8 A, Fig. 8 B, Fig. 8 C when water takes 6mL or 12mL, the mass change of gypsum and cement is in once
Functional relation, and have the part that can not be completely dissolved, when water is 9mL, the mass change of gypsum and cement is closed in quadratic function
System, and it is 9g in materials A, there is minimum point when being 5g in material B, i.e. setting time is most fast.Therefore in the proportioning of mixture, add
The water entered all will appear from the phenomenon that mixture is difficult to condense very little or too much.Very little, mixture is difficult to the ratio of its reclaimed water
Even stirring, your condensation product hardness and surface roughness be all difficult to be protected, and when water content is more than enough, will greatly increase
Mixture setting time, the hardness standard of printed material is unable to reach, in print procedure, printed part may be due to
It is also non-condensing and newly printed one layer and damage the generation for causing phenomena such as caving in.
In summary, with reference to the links such as the feeding of 3D printer, extrusion, printing to the setting time of printed material, hardness,
The requirement such as high temperature resistant, corrosion-resistant and surface roughness, combining response face method are matched to the analysis of experiments of rock-like materials,
That is gypsum 9.35g, cement 5g, water 6.12mL.
17 groups of different presetting periods of proportioning data, the theoretical value of final setting time and experiment are obtained by experiment above
Value, the analysis of the above is carried out to theoretical value and experiment value, according to center combination design, using the fit equation of quadratic function, is given
Go out following 21 kinds of prioritization schemes, wherein, A is the quality of gypsum, and unit is g, and B is the quality of cement, and unit is g, and C is the body of water
Product, Unit/mL, R1, R2 are respectively presetting period and final setting time, and unit is s, different ratio scheme lower setting time and expectation
Value is as shown in table 10.
The prioritization scheme list of table 10
With reference to requirement of the 3D printing technique to printed material, presetting period of printed material must be on the occasion of and can not mistake
Greatly, when being more than 3s in the presetting period, certain influence will be produced to the surface roughness of the precision of printing and printout, and printed
During requirement to final setting time it is more wide in range, it is maintained within 5s to print result all without producing excessive influence.
Therefore the selection wherein presetting period is shorter, and final setting time is reasonable, and also less six groups of desired value, (i.e. the first six group in Fig. 1
Data) the further verification experimental verification of optimization design progress, matched according to this six groups experiment, under equal conditions tested again,
Its result is as shown in table 11：
The checking test condition of table 11 and result
As can be seen from Table 11, the presetting period corresponding to this six groups of Optimal Parameters and final setting time and experiment are acquired
As a result very close, relative error illustrate that established model is accurate, reliably all 4% or so.Wherein the 6th group of experiment (stone
Cream 9.35g, cement 5g, water 6.12mL) presetting period is most short, it is expected minimum, although final setting time compared with first five items compared to it is long a bit,
But to print quality and have no significant effect, therefore the rock-like materials that final choice is formulated by the ratio are 3D printer
Printed material.
Claims (8)
1. a kind of screening technique of the rapid condensation proportioning of rock-like materials, it comprises the following steps：
(1) at least two materials are selected as detected materials according to general requirement of the 3D printing technique to material；
(2) combining response face method determines different experiment proportionings, i.e. ratio between detected materials and water, establishes response surface analysis
Model, and detected materials and water are mixed to get mixing material according to different experiment proportionings, 3D printing experiment is carried out respectively, is obtained
The measured value in presetting period, final setting time to the mixing material of different experiments proportioning；
With response surface design analyze method be fitted, obtain concentration of the detected materials in the mixing material with it is pre-hardening when
Between, the functional relation of final setting time, and then obtain presetting period, the predicted value of final setting time；
Establish different experiments proportioning the presetting period of mixture, the experiment value of final setting time and predicted value normal distribution,
Experimental analysis variogram, residual error and prognostic chart, prediction and actual figure, prediction and runtime value figure and the quality and water of detected materials
Volume between contour map, three-dimensional response surface design figure；
Pass through experimental analysis variogram, fitting quadratic regression equation, residual plot, predicted value figure, contour map, three-dimensional response surface design
Figure, optimize the value of the quality of detected materials and the volume of water, make its response in corresponding mapping range and export most
Small response；
Analyze the normal distribution, experimental analysis variogram, residual error and prognostic chart, prediction and actual figure, prediction and runtime value
Figure, and by experiment obtain the presetting period, final setting time experiment value, to the experiment value carry out response surface analysis, returned
Return model, and calculate presetting period, the theoretical value of final setting time, and obtain presetting period, the predicted value of final setting time with treating
Mutual functional relation between the quality of the functional relation and detected materials between the quality of material, the volume of water of measuring and monitoring the growth of standing timber；
(3) according to center combination design, with reference to the result obtained in step (2), using the fit equation of quadratic function to initial set
Time, final setting time are fitted, and the proportion optimizing scheme of detected materials and water and corresponding initial set are obtained according to fitting result
Time, final setting time, desired value；
(4) 3D printing experiment is carried out again according to the detected materials of the quality such as proportion optimizing scheme, selection and water, obtain optimization and match somebody with somebody
The experiment value in presetting period, final setting time than scheme, and by experiment value compared with the theoretical value, obtain relative miss
Difference, judge whether fitting is reasonable：If rationally, the selection wherein presetting period is most short, minimum it is expected, final setting time rational one assembles
Than the mixing material gone out with the proportional arrangement is the material of rock-like materials 3D printing；
If unreasonable, repeat step (3), until obtaining rational fitting result.
2. the method according to claim 11, wherein, in step (1), general requirement of the 3D printing technique to material
Including：
Be advantageous to fast, accurately process prototype parts；
Rapid shaping product should approach final requirement, meet the requirement to intensity, rigidity, moisture resistance, thermal stability；
Be advantageous to follow-up handling process.
3. according to the method for claim 1, wherein, the normal distribution for the detected materials studentized residuals with
The relation curve of mass percent, the studentized residuals are abscissa, and the mass percent is ordinate.
4. the method according to claim 11, wherein, the residual error and predicted value of the prognostic chart for the detected materials and
The relation curve of biochemical residual error, the residual error are ordinate, and the predicted value is abscissa.
5. the method according to claim 11, wherein, the prediction and the relation that actual figure is the predicted value and actual value
Curve, wherein, the predicted value is ordinate, and the actual value is abscissa.
6. according to the method for claim 1, wherein, the prediction and the studentization that runtime value figure is the detected materials are residual
The relation curve of difference and operation sequence number, the studentized residuals are ordinate, the operation serial number abscissa.
7. according to the method for claim 1, wherein, the 3D printing in the step (2) and step (4) is tested according to following
Step is carried out：
Various detected materials and water are weighed according to experiment proportioning；
Detected materials are mixed with water, obtain mixing material；
Mixing material is inserted to the extrusion device of 3D printer, stirred when inserting, prevents rocks class condensation of materials；
The extrusion device for installing mixing material is fixed on 3D printer, starts the reducing motor of printing, by mixing material from
Squeeze out in extrusion device, and heated on chassis, accelerate the rate of set of rock-like materials, be allowed to fast short-term training
Type, experiment is completed, in forming process, gathers the extruded velocity of mixing material, the heating-up temperature on chassis, presetting period, final set
Time.
8. a kind of rock-like materials 3D printing material, it is the proportioning obtained according to the method described in claim any one of 1-7
Prepare, the material includes gypsum, cement, water, and the ratio of three is 9.35g：5g：6.12mL.
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| CN103864376A (en) * | 2012-12-14 | 2014-06-18 | 梁三妹 | Artificial stone and preparation method thereof |
| CN104891891A (en) * | 2015-05-06 | 2015-09-09 | 同济大学 | 3D printing cement-based material and preparation method thereof |
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| CN103864376A (en) * | 2012-12-14 | 2014-06-18 | 梁三妹 | Artificial stone and preparation method thereof |
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