A data processing method for measuring wood microfibril angle based on XRD method

Abstract

The present invention discloses a data processing method for measuring the microfibril angle of wood based on the XRD method, and belongs to the technical field of wood microfibril angle detection. The data processing method for measuring the microfibril angle of wood based on the XRD method of the present invention comprises the following steps: the experimental sample is a wood core drilled from a growth cone with a diameter of 5 mm. In order to solve the problem that there is no unified standard for the data processing of the existing XRD test results, and it is difficult for beginners to calculate the microfibril angle based on a large amount of data, when the microfibril angle is measured by the XRD method, the original data is simulated by the Gauss equation to find the inflection point and the peak value, and a detailed and easy-to-understand microfibril angle data processing method is provided. Beginners can also perform relevant calculations according to this method. After becoming proficient, it only takes 5 minutes to process a set of data. In the process of processing data, important data information is retained to facilitate subsequent sorting and error correction. After becoming proficient, a set of data can be processed within 5 minutes.

Description

Technical Field

[0001] The invention relates to the technical field of wood microfibril angle detection, and in particular to a data processing method for measuring wood microfibril angle based on an XRD method. Background Art

[0002] The microfibril angle refers to the angle between the direction of the microfibrils in the S2 layer of the wood cell wall and the main axis of the cell. It is one of the indicators that directly determine the physical properties of wood and affects the processing and utilization of wood. In the process of analyzing wood properties, the microfibril angle is generally required to be measured. At present, the most commonly used method for measuring the microfibril angle of wood is X-ray diffraction (XRD). This method is rapid, reproducible, and representative, and is particularly suitable for variation studies of a large number of samples.

[0003] However, there is no unified standard for the data processing of existing XRD test results, and it is difficult for beginners to calculate the microfibril angle based on a large amount of data; therefore, it does not meet the existing needs. In this regard, we propose a data processing method for determining the microfibril angle of wood based on the XRD method. Summary of the invention

[0004] The purpose of the present invention is to provide a data processing method for determining the microfibril angle of wood based on the XRD method, to search for inflection points and peak values ​​after simulating the original data with the Gauss equation, and to provide a detailed and easy-to-understand microfibril angle data processing method. Beginners can also perform relevant calculations according to this method. After becoming proficient, it only takes 5 minutes to process a set of data. During the data processing, important data information is retained to facilitate subsequent sorting and error correction. After becoming proficient, a set of data can be processed within 5 minutes, which can solve the problems in the prior art.

[0005] To achieve the above object, the present invention provides the following technical solution: a data processing method for measuring wood microfibril angle based on XRD method, characterized in that it comprises the following steps:

[0006] A data processing method for measuring wood microfibril angle based on XRD method comprises the following steps:

[0007] Step 1: The experimental sample is a wood core drilled from a 5mm diameter growth cone. Use a knife to cut thin slices with a thickness of 1-2mm. The surface must be smooth and dried in a 60℃ oven until absolutely dry before subsequent testing.

[0008] Step 2: Use double-sided tape to fix the test sample on the sample rotating table, and install the sample rotating table on the instrument;

[0009] Step 3: Use Origin 2021 software to process the data, copy the result data into a table, and select two columns of data:

[0010] Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph1";

[0011] Select "Graph1":

[0012] First, click the "Quick Analysis" option, and then click "Quick Fit" again in the option to finally generate Peak-Gauss (System);

[0013] Step 4: Stretch the yellow box to the left and right to cover the entire line chart, then create a new output, record the y0, xc, w, and A parameters in the result log into a table, and select the C and D columns of data:

[0014] Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph2";

[0015] Select "Graph2":

[0016] Click the "Analysis" option in the toolbar, expand it and select "Mathematics", then select "Differential" in the sub-unit options, and click "Open Dialog" to set the "Derivative Order" to "2", click OK, and the "E(Y2)" column will appear in "Book1";

[0017] Step 5: Right-click the blank space of "Book1", click "Add New Column", fill the new column F(Y2) with 0, and select columns E(Y2) and F(Y2):

[0018] Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph3";

[0019] Select "Graph3":

[0020] Click to expand the "Quick Analysis" option, then select the "Intersection" function option, click OK directly, click "New Output", and record the horizontal coordinates of the two intersection points;

[0021] Step 5: Select "Graph2", click Tangent plug-in, use default parameters, move the red vertical line, make the horizontal coordinate of the tangent point as close as possible to the inflection point (X1), record the tangent point coordinates and tangent equation in the table, similarly, make a tangent line at another inflection point, and record the tangent point coordinates and tangent equation;

[0022] Step 6: Select "Graph2":

[0023] Click the "Analysis" option in the toolbar, expand it and select "Peak and Baseline", then select "Peak Analysis", and click "Open Dialog", click Next, set "Baseline Mode" to "Constant", select "Minimum", and record the value of Y at this time;

[0024] Calculate the intersection points of the baseline with tangent 1 and tangent 2, substitute Y into the straight line equations, and record them;

[0025] Microfibril angle MAF=(x2-x1) / 2*0.6.

[0026] Preferably, in step 2, the instrument setting parameters are: tube voltage 40 kV, tube current 30 mA, scanning speed 72° / min, and the range of the sample rotating table (1) is 90°~270°.

[0027] Preferably, in step 2, both ends of the surface of the sample rotating table are provided with pad shaft seat grooves, and the pad shaft seat grooves are provided inside with supporting pad shafts, both sides of the surface of the sample rotating table are provided with supporting slide grooves, and both ends of the supporting slide grooves are provided with sample clamps, and one end of the sample rotating table is provided with a table plate assembly groove.

[0028] Preferably, the sample clamp is slidably connected to the support slide, and a slide sleeve is provided above the sample clamp, the slide sleeve is fittedly connected to the sample clamp, and the slide sleeve is connected to the sample rotating table by screws.

[0029] Preferably, a stop groove is provided on one side of the sample clamp, and a movable knob is provided inside the stop groove, the movable knob is rotatably connected to the sample clamp, and a displacement screw is provided between the movable knob and the support pad shaft.

[0030] Preferably, the shift screw and the movable knob are rotationally connected via a bearing, and the shift screw and the support pad shaft are rotationally connected via an internal thread, a locking screw is provided at the top of the support pad shaft, and the locking screw extends through to the bottom of the support pad shaft.

[0031] Preferably, in step three, the experimental result data is saved in "txt" and "raw" formats, and the data needs to be saved after each sample is tested.

[0032] Preferably, in the step 4,

[0033] The parameters of sample number 1 are: y0=1029.57, xc=182.137, w=50.8445, A=31416.7;

[0034] The parameters of sample number 2 are: y0=654.5199, xc=187.2874, w=32.58595, A=29222.92.

[0035] Preferably, in step five,

[0036] The parameters of sample number a are: X1=156.714, X2=207.5599;

[0037] The parameters of sample number b are: X1=170.9935, X2=203.5813.

[0038] Preferably, in step five,

[0039] The parameters of sample number c are: tangent point X1=156.6667, tangent point X2=207.4775, tangent point Y2=1329.561;

[0040] The parameters of sample number d are: cut point X1=171.0811, cut point X2=203.6937, cut point Y2=1085.498.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] 1. The present invention uses XRD method to measure microfibril angle. Different from the conventional 2cm*2cm wood slice sample, this method is simple to prepare and uses less sample. The nanny-level data processor uses Origin software to simulate the original data with Gauss equation and then find the inflection point and peak value, providing a detailed and easy-to-understand microfibril angle data processing method. Beginners can also perform relevant calculations according to this method. After becoming proficient, it only takes 5 minutes to process a set of data. In the process of processing data, important data information is retained to facilitate subsequent sorting and error correction. After becoming proficient, a set of data can be processed within 5 minutes;

[0043] 2. The present invention, when in use, places the sample between two sets of sample clamps, and then rotates the movable knob inside the sample clamp to rotate the shift screw, and the shift screw can be extended and retracted with the support pad shaft as a fulcrum, so that the movement function of the sample clamp can be controlled, thereby fixing the sample;

[0044] 3. In the present invention, a locking screw is provided on the top of the support pad shaft, and the locking screw extends through to the bottom of the support pad shaft. The support pad shaft can be locked inside the pad shaft seat groove by rotating the locking screw, thereby preventing the support pad shaft from offsetting and sliding during the process of fixing the sample material. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 It is the line graph of Graph1 of the present invention;

[0046] Figure 2 It is the Graph2 line graph of the present invention;

[0047] Figure 3 It is a sequence framework diagram of the present invention;

[0048] Figure 4 It is the Graph3 line graph of the present invention;

[0049] Figure 5 It is the tangent point line graph of Graph2 of the present invention;

[0050] Figure 6 The schematic diagram of the baseline equation structure of the present invention is

[0051] Figure 7 It is a schematic diagram of the structure of the sample rotating table of the present invention.

[0052] In the figure: 1, sample rotating table; 2, slide plate; 3, support shaft; 4, sample clamp; 101, shaft seat groove; 102, table assembly groove; 103, support slide groove; 301, shift screw; 302, movable knob; 303, locking screw knob; 401, positioning groove. DETAILED DESCRIPTION

[0053] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0054] See also Figure 1-6 An embodiment of the present invention provides a data processing method for measuring wood microfibril angle based on XRD method, characterized in that it comprises the following steps:

[0055] Step 1: The experimental sample is a wood core drilled from a 5mm diameter growth cone. Thin slices with a knife are cut to a thickness of 1~2mm. The surface must be smooth. After drying in a 60℃ oven until absolutely dry, subsequent tests are performed. The original data obtained after measuring the wood microfibril angle by XRD method are the test setting parameters and 71 rows and 2 columns of values. Most of the literature simply replaces the data processing method, and it is difficult for beginners to calculate the microfibril angle based on a large amount of data. Based on the 0.6T method, the original data is simulated by the Gauss equation using Origin software to find the inflection point and peak value. A detailed and easy-to-understand microfibril angle data processing method is provided. Beginners can also perform relevant calculations based on this method. After becoming proficient, it only takes 5 minutes to process a set of data;

[0056] Step 2: Use double-sided tape to fix the test sample on the sample rotating table 1, and install the sample rotating table 1 on the instrument;

[0057] Step 3: Use Origin 2021 software to process the data, copy the result data into a table, and select two columns of data:

[0058] Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph1";

[0059] Select "Graph1":

[0060] First, click the "Quick Analysis" option, and then click "Quick Fit" again in the option to finally generate Peak-Gauss (System);

[0061] Step 4: Stretch the yellow box to the left and right to cover the entire line chart, then create a new output, record the y0, xc, w, and A parameters in the result log into a table, and select the C and D columns of data:

[0062] Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph2";

[0063] Select "Graph2":

[0064] Click the "Analysis" option in the toolbar, expand it and select "Mathematics", then select "Differential" in the sub-unit options, and click "Open Dialog" to set the "Derivative Order" to "2", click OK, and the "E(Y2)" column will appear in "Book1";

[0065] Step 5: Right-click the blank space of "Book1", click "Add New Column", fill the new column F(Y2) with 0, and select columns E(Y2) and F(Y2):

[0066] Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph3";

[0067] Select "Graph3":

[0068] Click to expand the "Quick Analysis" option, then select the "Intersection" function option, click OK directly, click "New Output", and record the horizontal coordinates of the two intersection points;

[0069] Step 5: Select "Graph2", click Tangent plug-in, use default parameters, move the red vertical line, make the horizontal coordinate of the tangent point as close as possible to the inflection point (X1), record the tangent point coordinates and tangent equation in the table, similarly, make a tangent line at another inflection point, and record the tangent point coordinates and tangent equation;

[0070] Step 6: Select "Graph2":

[0071] Click the "Analysis" option in the toolbar, expand it and select "Peak and Baseline", then select "Peak Analysis", and click "Open Dialog", click Next, set "Baseline Mode" to "Constant", select "Minimum", and record the value of Y at this time;

[0072] Calculate the intersection points of the baseline with tangent 1 and tangent 2, substitute Y into the straight line equations, and record them;

[0073] Microfibril angle MAF=(x2-x1) / 2*0.6.

[0074] In step 2, the instrument setting parameters are: tube voltage 40 kV, tube current 30 mA, scanning speed 72° / min, and sample rotation stage (1) range 90°~270°.

[0075] In step three, the experimental result data is saved in "txt" and "raw" formats, and the data needs to be saved after each sample is tested.

[0076] In step four,

[0077] The parameters of sample number 1 are: y0=1029.57, xc=182.137, w=50.8445, A=31416.7;

[0078] The parameters of sample number 2 are: y0=654.5199, xc=187.2874, w=32.58595, A=29222.92.

[0079] In step five,

[0080] The parameters of sample number a are: X1=156.714, X2=207.5599;

[0081] The parameters of sample number b are: X1=170.9935, X2=203.5813.

[0082] In step five,

[0083] The parameters of sample number c are: tangent point X1=156.6667, tangent point X2=207.4775, tangent point Y2=1329.561;

[0084] The parameters of sample number d are: cut point X1=171.0811, cut point X2=203.6937, cut point Y2=1085.498.

[0085] See also Figure 7, both ends of the surface of the sample rotating table 1 are provided with a pad shaft seat groove 101, and the pad shaft seat groove 101 is provided with a supporting pad shaft 3 inside, both sides of the surface of the sample rotating table 1 are provided with a supporting slide groove 103, and both ends of the supporting slide groove 103 are provided with a sample clamping plate 4, one end of the sample rotating table 1 is provided with a table plate assembly groove 102, the table plate assembly groove 102 is located at one end of the sample rotating table 1, and its main function is to facilitate the installation and fixing operation between the sample rotating table 1 and the diffractometer equipment, the sample clamping plate 4 is slidably connected with the supporting slide groove 103, and the sample is placed between the two groups of sample clamping plates 4 when in use, and then the movable knob 302 on the inner side of the sample clamping plate 4 is rotated to rotate the shift screw rod 301, and the shift screw rod 301 can realize the telescopic operation with the supporting pad shaft 3 as the fulcrum, so that the movement function of the sample clamping plate 4 can be controlled, thereby completing the fixation of the sample, and the sample A slide sleeve 2 is arranged above the clamping plate 4, the slide sleeve 2 is fitted and connected with the sample clamping plate 4, and the slide sleeve 2 is connected to the sample rotating table 1 by screws, a stop groove 401 is arranged on one side of the sample clamping plate 4, and a movable knob 302 is arranged inside the stop groove 401, the movable knob 302 is rotatably connected with the sample clamping plate 4, and a shift screw 301 is arranged between the movable knob 302 and the support pad shaft 3, the shift screw 301 is rotatably connected with the movable knob 302 through a bearing, and the shift screw 301 is rotatably connected with the support pad shaft 3 through an internal thread, a locking screw 303 is arranged on the top of the support pad shaft 3, and the locking screw 303 extends through and extends to the bottom of the support pad shaft 3, the support pad shaft 3 can be locked inside the pad shaft seat groove 101 by rotating the locking screw 303, so as to avoid the support pad shaft 3 from offsetting and sliding during the process of fixing the sample material.

[0086] In summary, the experimental samples are wood cores drilled from growth cones with a diameter of 5 mm. Different single plant samples are prepared from the same annual ring as much as possible. Thin slices are cut with a knife, with a thickness of 1-2 mm and a smooth surface. They are dried in an oven at 60°C until absolutely dry before subsequent testing. In this experiment, an X-ray diffractometer is used to test the wood core samples. Double-sided tape is used to fix the test samples on the sample rotating table 1, and the sample rotating table 1 is installed on the instrument. When using, the sample is placed between two sets of sample clamps 4, and then the movable knob 302 on the inner side of the sample clamp 4 is turned. The shift screw 301 is rotated to realize telescopic operation with the support shaft 3 as the fulcrum, so that the movement function of the sample clamp 4 can be controlled, so as to fix the sample. A locking screw 303 is arranged on the top of the support shaft 3, and the locking screw 303 extends through and extends to the bottom of the support shaft 3. The support shaft 3 can be locked in the shaft seat groove 101 by rotating the locking screw 303, so as to avoid the support shaft 3 from sliding in the process of fixing the sample material. 2021 software for data processing, copy the result data into the table, select two columns of data, right-click on the current page and select Drawing, then choose to generate a line graph to get "Graph1", select "Graph1", first click the "Quick Analysis" option, click "Quick Fit" again in the option to finally generate Peak-Gauss (System), stretch the yellow box to the left and right to cover the entire line graph, then create a new output, record the y0, xc, w, and A parameters in the result log into the table, select the C and D columns of data, right-click on the current page and select Drawing, then choose to generate a line graph to get "Graph2", select "Graph2", click the "Analysis" option on the toolbar, expand it and select "Mathematics", then select "Differential" in the subunit option, and click "Open Dialog Box" to set the "Order of Derivative" to "2", click OK, and the "E(Y2)" column will appear in "Book1", right-click In the blank space of "Book1", click "Add New Column" and fill 0 in the new column F(Y2). Select the E(Y2) and F(Y2) columns. Right-click on the current page and select Drawing. Then select Generate Line Graph to get "Graph3". Select "Graph3", click to expand the "Quick Analysis" option, and then select the "Intersection" function option. Click OK directly. Click "New Output" to record the horizontal coordinates of the two intersection points. Select "Graph2", click the Tangent plug-in, use the default parameters, move the red vertical line, and make the horizontal coordinate of the tangent point as close to the inflection point (X1) as possible. Record the tangent coordinates and tangent equation at this time in the table. Similarly, make a tangent at another inflection point, and record the tangent coordinates and tangent equation. Select "Graph2", click the "Analysis" option on the toolbar, expand and select "Peak and Baseline", then select "Peak Analysis", and click "Open Dialog" at the same time. Click Next, and set "Baseline Mode" to "Constant".Select "Minimum", record the value of Y at this time, calculate the intersection of the baseline with tangent 1 and tangent 2 at this time, substitute Y into the straight line equation, and record.

[0087] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0088] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A data processing method for measuring wood microfibril angle based on XRD method, characterized in that: The steps include: Step 1: The experimental sample is a wood core drilled from a 5 mm diameter growth cone. Use a knife to cut thin slices with a thickness of 1 to 2 mm. The surface must be smooth and dried in a 60°C oven until absolutely dry before subsequent testing. Step 2: Use double-sided tape to fix the test sample on the sample rotating table (1), and install the sample rotating table (1) on the instrument; Step 3: Use Origin 2021 software to process the data, copy the result data into a table, and select two columns of data: Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph1"; Select "Graph1": First, click the "Quick Analysis" option, and then click "Quick Fit" again in the option to finally generate Peak-Gauss (System); Step 4: Stretch the yellow box to the left and right to cover the entire line chart, then create a new output, record the y0, xc, w, and A parameters in the result log into a table, and select the C and D columns of data: Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph2"; Select "Graph2": Click the "Analysis" option in the toolbar, expand it and select "Mathematics", then select "Differential" in the sub-unit options, and click "Open Dialog" to set the "Derivative Order" to "2", click OK, and the "E(Y2)" column will appear in "Book1"; Step 5: Right-click a blank space in "Book1", click "Add New Column", fill the new column F(Y2) with 0, and select columns E(Y2) and F(Y2): Right-click on the current page and select Draw, then select Generate Line Graph to get "Graph3"; Select "Graph3": Click to expand the "Quick Analysis" option, then select the "Intersection" function option, click OK directly, click "New Output", and record the horizontal coordinates of the two intersection points; Step 5: Select "Graph2", click Tangent plug-in, move the red vertical line so that the horizontal coordinate of the tangent point is as close to the inflection point as possible, record the tangent point coordinates and tangent equation in the table. Similarly, make a tangent line at another inflection point and record the tangent point coordinates and tangent equation. Step 6: Select "Graph2": Click the "Analysis" option in the toolbar, expand it and select "Peak and Baseline", then select "Peak Analysis", and click "Open Dialog", click Next, set "Baseline Mode" to "Constant", select "Minimum", and record the value of Y at this time; Calculate the intersection points of the baseline with tangent 1 and tangent 2, substitute Y into the straight line equations, and record them; Microfibril angle MAF = (x2-x1) / 2*0.

6.

2. The data processing method for measuring wood microfibril angle based on XRD method according to claim 1, characterized in that: In step 2, the instrument setting parameters are: tube voltage 40 kV, tube current 30 mA, scanning speed 72° / min, and the range of the sample rotating table (1) is 90° to 270°.

3. The data processing method for measuring wood microfibril angle based on XRD method according to claim 1, characterized in that: In the step 2, both ends of the surface of the sample rotating table (1) are provided with axle seat grooves (101), and a supporting axle (3) is provided inside the axle seat grooves (101), both sides of the surface of the sample rotating table (1) are provided with supporting slide grooves (103), and both ends of the supporting slide grooves (103) are provided with sample clamps (4), and one end of the sample rotating table (1) is provided with a table assembly groove (102).

4. The data processing method for measuring wood microfibril angle based on XRD method according to claim 3, characterized in that: The sample clamping plate (4) is slidably connected to the supporting slide groove (103), and a slide groove sleeve plate (2) is arranged above the sample clamping plate (4), the slide groove sleeve plate (2) is closely connected to the sample clamping plate (4), and the slide groove sleeve plate (2) is connected to the sample rotating platform (1) by screws.

5. The data processing method for measuring wood microfibril angle based on XRD method according to claim 4, characterized in that: A stop groove (401) is provided on one side of the sample clamping plate (4), and a movable knob (302) is provided inside the stop groove (401); the movable knob (302) is rotatably connected to the sample clamping plate (4), and a displacement screw (301) is provided between the movable knob (302) and the support pad shaft (3).

6. The data processing method for measuring wood microfibril angle based on XRD method according to claim 5, characterized in that: The shift screw (301) is rotatably connected to the movable knob (302) via a bearing, and the shift screw (301) is rotatably connected to the support pad shaft (3) via an internal thread. A locking screw button (303) is provided at the top of the support pad shaft (3), and the locking screw button (303) extends through and extends to the bottom of the support pad shaft (3).

7. The data processing method for measuring wood microfibril angle based on XRD method according to claim 1, characterized in that: In step three, the experimental result data is saved in "txt" and "raw" formats, and the data needs to be saved after each sample is tested.

Images