JP3344384B2 - Method for measuring viscosity of green compact, viscosity measuring device for green compact, and computer-readable recording medium recording viscosity measuring method for green compact - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the viscosity of a green compact formed by press-molding crystallized glass powder and the like, a device for measuring the viscosity of a green compact, and the viscosity of a green compact. The present invention relates to a computer-readable recording medium on which a measurement method is recorded.

[0002]

2. Description of the Related Art In recent years, in the electronics industry, research and development of ceramic multilayer substrates and thick film materials capable of coping with high-density mounting and high frequency have been actively conducted. In particular, a low-temperature sintered ceramic multilayer substrate made of an amorphous glass powder or a crystallized glass powder has a small relative dielectric constant and can be co-fired with a conductive material such as Ag having a small specific resistance, so that it has various electrical characteristics. It can be an excellent ceramic multilayer substrate.

In such ceramic multilayer substrates and thick film materials, the physical properties of oxide inorganic powders such as amorphous glass powder and crystallized glass powder greatly contribute to substrate characteristics and thick film characteristics. Above all, the viscosity characteristics greatly affect the sintering process of the oxide inorganic powder, the diffusion behavior of the Ag conductor, and the like, and are extremely important parameters in material design and process design.

[0004]

Generally, the viscosity of these glass powders is about 10 ¹⁰ Pa · S or more in a high viscosity region of about 10 ⁴ Pa · S
The following low viscosity regions are measured by a rotary viscometer (sphere pulling viscometer). In the sintering process of these glass powders, 10 ⁴ to 10 ⁹ Pa
In the medium viscosity region of S, viscosity measurement using a parallel plate pressure viscometer is performed.

Hereinafter, a method of measuring the viscosity η using a parallel plate pressure viscometer will be described.

First, as shown in FIG. 15, an object (sample) 1 whose height H and volume V are accurately measured is placed on a quartz plate 2a fixed to a support table 3. Then
After being sandwiched by a quartz plate 2b fixed to the quartz rod 4, a constant load M is applied to the quartz rod 4 and the temperature inside the device 6 is increased by the heater 5, and the differential transformer (shown in FIG. (Omitted), the displacement (height H) of the DUT 1 is detected. Then, by extracting this displacement with time, the sample deformation speed dh / d of the DUT 1 is obtained.
Calculate t.

Next, the volume V of the object to be measured, the sample volume V, the load M, and the sample deformation speed dh / dt are calculated using the GENT equation: η = 2πMGH ⁵ / 3V (dh / dt) (2πH ³ + V) , M: load, H: sample height, G: gravitational acceleration,
V: sample volume, dh / dt: sample deformation rate) to calculate the viscosity η of the DUT 1 (ANGENT, BR)
ITISH JOURNAL OF APPLIED PHYSICS VOL.11, FEBRUARY
1960). This is performed for each temperature to derive a change in viscosity η with temperature, that is, a viscosity-temperature curve.

However, in the above-described viscosity measurement using a parallel plate pressure viscometer, it is necessary to use a bulk sample as the DUT 1. In other words, the GENT formula is a viscosity conversion formula that is established when the DUT 1 can be assumed to be an incompressible fluid. For example, when measuring the viscosity of glass powder, the glass powder is melted, quenched, and bulk-cooled. Molded bulk samples must be used.

[0009] That is, in the above-mentioned method, it is possible to measure the viscosity of glass molded into a bulk, but it is difficult to measure the viscosity of glass in a powder state, particularly crystallized glass powder. This is because a crystallized glass powder having a strong tendency to crystallize may precipitate crystals during the preparation of a bulk sample. Even if a bulk sample can be produced, the crystallization behavior is essentially different between the bulk sample and the powder sample. The difference appears.

However, as described above, in the case of ceramic multilayer substrates and thick film materials, crystallized glass, amorphous glass, and the like are mostly used as powder samples. That is, in the material design and the process design, it is necessary to evaluate the viscosity characteristics of a crystallized glass, an amorphous glass, and the like as a powder sample.

The present invention has been made in view of the above circumstances, and has as its object to measure the viscosity of a green compact formed by press-molding an inorganic powder with high accuracy. It is to provide a measuring method. Still another object of the present invention is a device for measuring the viscosity of a green compact, which can efficiently measure the viscosity of a green compact, and a computer-readable recording medium that records a method for measuring the viscosity of a green compact. To provide.

[0012]

That is, according to the present invention, the viscosity η of a green compact formed by press-molding an inorganic powder is defined as G
ENT formula: η = 2πMGH ⁵ / 3V (dh / dt) (2πH ³ + V) (However, M: load, H: sample height, G: gravity acceleration,
V: sample volume, dh / dt: sample deformation rate), which is a method for measuring the viscosity of a green compact,
(A) determining a sample volume correction value V ′ of the green compact (where the sample volume correction value V ′ is the volume occupied by the inorganic powder in the green compact); The sample deformation speed correction value (dh / dt) 'of the molded body (where the sample deformation speed correction value (dh / dt)' is the difference between the apparent sample deformation speed and the sample deformation speed due to sintering shrinkage) Step, (C) Displacement of the green compact,
A step of separating a temperature region X in which sintering shrinkage is dominant and a temperature region Y in which plastic deformation is dominant; (D) The temperature region X in which sintering shrinkage is dominant is defined as a sample volume V of the GENT formula. Applying the sample volume correction value V 'and applying the sample deformation speed correction value (dh / dt)' as the sample deformation speed dh / dt; (E) the temperature region Y in which the plastic deformation is dominant. About the GE
Applying the sample volume correction value V ′ as the NT type sample volume V 1.

According to the method of measuring the viscosity of a green compact according to the present invention, (A) correction of sample volume → correction value of sample volume for viscosity measurement conventionally applicable only to incompressible fluids such as bulk samples. Extraction step of V ′ (B) Correction of sample deformation speed → Extraction step of sample deformation speed correction value (dh / dt) ′ (C) Regarding displacement of the green compact, temperature range X, where sintering shrinkage is dominant, The separation step of the temperature region Y where the plastic deformation is dominant is executed.
(D) In the temperature region X where sintering shrinkage is dominant, the sample volume is corrected and the sample deformation rate is corrected. (E) In the temperature region Y where the plastic deformation is dominant, the sample volume is extremely corrected by executing the sample volume correction. It is possible to measure the viscosity of a compact having a similar viscous behavior with high accuracy.

Further, in the present invention, the viscosity η of a green compact formed by press-molding an inorganic powder is determined by the GENT equation: η = 2πMGH ⁵ / 3V (dh / dt) (2πH ³ + V) (where M: Load, H: sample height, G: gravitational acceleration,
V: a sample volume, dh / dt: sample deformation rate), which is a device for measuring the viscosity of a green compact,
(A) a sample shape measuring unit for measuring an actual measured value of the shape of the green compact; (b) a sample deformation speed measuring unit for measuring an apparent sample deformation speed of the green compact; (c) the green compacting An arithmetic processing means for calculating a volume occupied by the inorganic powder in the green compact based on the actual measured value of the body shape, and outputting the calculated volume as a sample volume correction value V '; (d) the apparent sample deformation speed A calculating means for calculating a difference between a sample deformation speed due to sintering shrinkage of the green compact and a sample deformation speed correction value (dh / dt) 'of the green compact;
(E) With respect to the displacement of the green compact, arithmetic processing means for determining a boundary temperature between a temperature region X in which sintering shrinkage is dominant and a temperature region Y in which plastic deformation is dominant, (f) the sintering shrinkage is For the dominant temperature region X, the sample volume correction value V ′ is applied as the sample volume V 1 of the GENT equation, and the sample deformation speed correction value (dh / dt) ′ is used as the sample deformation speed dh / dt. By applying, the arithmetic processing means for outputting the viscosity η in the temperature region X; (g) For the temperature region Y in which the plastic deformation is dominant, the GEN
The viscosity η in the temperature region Y is output by applying the sample volume correction value V ′ as the sample volume V of the T formula.
A viscosity measuring device for a green compact, comprising: (h) a display unit for displaying the viscosity η in the temperature region X and the viscosity η in the temperature region Y. is there.

According to the apparatus for measuring the viscosity of a green compact of the present invention, there are provided (a) a sample shape measuring section, and (b) a sample deformation rate measuring section, and further, based on measured values from these measuring sections,
(C) Correction of sample shape → Extraction of sample volume correction value V ′ (d) Correction of sample deformation speed → Sample deformation speed correction value (dh
(E) Separation of temperature region X where sintering shrinkage is dominant and temperature region Y where plastic deformation is dominant (f) In temperature region X where sintering shrinkage is dominant, sample GENT equation (G) In the temperature region Y where plastic deformation is dominant, each temperature processing unit is provided with each processing means for performing the sample volume correction for the GENT equation, and the result of this processing, that is, ( h) Since the display unit for displaying the viscosity η of the green compact in each temperature range is provided, the powder state can be obtained by using the GENT equation, which was conventionally applicable only to incompressible fluids such as bulk samples. It is possible to efficiently measure the viscosity of a compact having a viscous behavior very close to that of a compact.

Further, the present invention provides a computer-readable recording program for recording the method for measuring the viscosity of a green compact, characterized by recording a program for causing a computer to execute the method for measuring the viscosity of a green compact according to the present invention. It provides a medium.

According to the computer-readable recording medium on which the method for measuring the viscosity of a green compact according to the present invention is recorded, a program for causing a computer to execute the method for measuring the viscosity of a green compact according to the present invention is recorded. The method for measuring the viscosity of a green compact according to the present invention can be stored, and the technology can be easily transferred, so that many people can use it easily.

[0018]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the method for measuring the viscosity of a green compact according to the present invention will be described in detail.

In general, in a viscosity measuring method using a parallel plate pressure viscometer, a sample viscosity η of a volume V is calculated by the following GENT formula.

Η = 2πMGH ⁵ / 3V (dh / dt)
(2πH ³ + V) (However, M: load, H: sample height, G: gravitational acceleration,
V: sample volume, dh / dt: sample deformation rate) FIG. 1 is a schematic view of a bulk sample and a compact of a SiO ₂ —B ₂ O ₃ —Al ₂ O ₃ —CaO-based crystallized glass powder described later. It is a viscosity-temperature curve at the time of applying a GENT formula. In addition, in FIG. 1, the bulk sample
It was melted at 650 ° C., kept at 650 ° C. for 30 minutes in a slow cooling furnace, and then gradually cooled at a rate of 2 ° C./min. On the other hand,
The green compact is obtained by press-molding the crystallized glass powder together with an organic vehicle.

As can be seen from FIG. 1, simply applying the sample deformation rate and the sample volume by the parallel plate pressure viscometer to the GENT equation, the viscosity-temperature curve of the bulk sample and the viscosity- Does not match temperature curve.
That is, despite the viscosity measurement of the same type of crystallized glass powder, it is observed that the bulk sample and the powder sample have significantly different viscosity behavior.

First, a viscosity increase is observed at around 830 ° C. in a green compact, but not in a bulk sample.
This increase in viscosity is mainly due to the difference in the easiness of crystallization between the green compact and the bulk sample. That is, as can be seen from the results of the thermal analysis (DSC analysis) shown in Table 1 below, both the crystallization onset temperature (Tc) and the crystallization peak temperature (Tcp) are 150 for the green compact compared to the bulk sample. About 160 to 160 ° C.

[0023]

[Table 1]

This is because the powder compact has a larger specific surface area than that of the bulk sample, so that crystallization (= nucleation and growth of crystal phase) from the crystallized glass powder surface is easily promoted. As a result, the crystallization temperature is shifted to a lower temperature side.

Next, FIG. 1 shows that the viscosity of the green compact was
Temperature curve is almost entirely viscosity by bulk sample - is far below than the temperature curve, also viscosity 10 ⁷ Pa
-It can be seen that, in the region of lower viscosity than near s, the viscosity-temperature curve of the bulk sample is close to but lower than the viscosity curve.

As described above, the GENT equation is a viscosity conversion equation that is established when an object to be measured can be assumed to be an incompressible fluid. On the other hand, in the case of a green compact formed by press-molding an inorganic powder and a vehicle, the volume changes due to sintering shrinkage and the like occur as the firing proceeds. Can not.

That is, simply as in the case of the bulk sample, the measurement data of the green compact is applied to the GENT equation, and the result cannot be used to determine the viscosity of the green compact. In order to be applicable to a green compact, the parameters in the GENT equation must be corrected.

For this purpose, first, in order to correct a substantial difference in volume between the bulk sample and the green compact,
The volume obtained by multiplying the apparent volume of the green compact by the filling rate of the crystallized glass powder in the green compact is defined as a sample volume correction value V ′, and this V ′ is applied to the GENT equation. Incidentally, the filling rate of the crystallized glass powder, the powder specific gravity of the crystallized glass powder,
It can be easily calculated from the mixing ratio and the weight of the green compact.

For example, as shown in the flowchart of FIG. 2, the weight m ₁ of the inorganic powder such as crystallized glass, the true specific gravity n ₁ ,
Sample weight m of the green compact, formulated amount w ₁ of the inorganic powder, to measure the compounding amount w ₂ of vehicle components, in accordance with the following equation, it is possible to calculate the sample volume correction value V '.

V ′ = m1 / n1, m1 = m × ｛w1 /
(W1 + w2)｝ Secondly, in the temperature region where sintering shrinkage is dominant in the displacement of the green compact, it is necessary to consider the sample deformation speed due to sintering shrinkage. That is, as shown in FIG. 3, the apparent sample deformation rate of the green compact includes the sample deformation rate due to plastic deformation and the sample deformation rate due to sintering shrinkage. , The sample deformation speed that compensates for it, ie, the sample deformation speed correction value (dh / d
t) 'must be applied to the GENT equation.

Here, as shown in FIG. 3, in the temperature region X where sintering shrinkage is dominant, the sample deformation rate (d
h / dt) ₀ can be regarded as the sample deformation rate accompanying sintering shrinkage. Therefore, in order to derive the sample deformation speed in the temperature region X, the sample deformation speed (dh / dt) ₀ at zero load may be calculated.

Sample deformation speed at zero load (dh / dt)
₀ is a sample deformation speed (dh / dt) when a load is shaken, as shown in FIG. 3, such as load A, load B,.
_A , (dh / dt) _B ... Were measured, and the value extrapolated to zero load was assumed for the sample at zero load, assuming that the relationship between the load at each temperature and the sample deformation rate could be linearly approximated. The deformation speed (dh / dt) is calculated as ₀ .

Specifically, as shown in the flow chart of FIG. 4, a load A at a temperature T ₁ is applied to the green compact.
Sample deformation rate at (dh / dt) _A, to measure the sample deformation rate (dh / dt) _B at load B. By executing the linear fit according to the least square method using the sample deformation rate (dh / dt) _A at load A, the sample deformation rate (dh / dt) _B at load B, when the temperatures T ₁ Calculate the sample deformation speed (dh / dt) ₀ at zero load.

Similarly, the sample deformation speed (dh / dt) ₀ at zero load at the temperatures T ₂ , T _3, ...
As shown in FIG. 5, a sample deformation speed-temperature curve ((dh / dt) ₀ -T curve) at zero load is prepared. A sample deformation speed-temperature curve under load A and a sample deformation speed-temperature curve under load B were prepared. From these curves, a sample deformation speed-temperature curve at zero load ((dh / dt) ₀ -T Curve) can be calculated at once.

Next, as shown in the flow chart of FIG. 4, a sample deformation speed correction value (dh / dt) ′ to be applied to the temperature region X where sintering shrinkage is dominant is calculated. The sample deformation speed correction value (dh / dt) 'can be calculated by taking the difference between the apparent sample deformation speed and the sample deformation speed accompanying sintering shrinkage.

Specifically, it is an apparent sample deformation speed.
Sample deformation rate under load A (dh / dt)_AOr load
Sample deformation speed at B (dh / dt)_BFrom sintering shrinkage
The sample deformation speed at zero load, which is the sample deformation speed (d
h / dt)₀Is subtracted from the sample deformation speed correction value (d
h / dt) '. This operation is performed at the temperature T
₁, T_Two, T_Three…, Deformation of the sample at each temperature
The speed correction value (dh / dt) 'is calculated.

Further, as shown in the flowchart of FIG. 4, a temperature region X in which sintering shrinkage is dominant and a temperature region Y in which plastic deformation is dominant are separated. This separation is caused by the sample deformation rate-temperature curve ((dh /
dt) ₀ -T curve).

Specifically, as shown in FIG. 5, the minimum value in the sample deformation speed-temperature curve ((dh / dt) ₀ -T curve) at zero load is regarded as its boundary temperature Tb, A temperature region lower than Tb is defined as a temperature region X in which sintering shrinkage is dominant, and a temperature region higher than the boundary temperature Tb is defined as a temperature region Y in which plastic deformation is dominant.

As shown in FIG. 6, with respect to the displacement of the green compact, in the temperature region X where sintering shrinkage is dominant, G
Regarding the ENT equation, sample volume V → sample volume correction value V ′ sample deformation speed dh / dt → sample deformation speed correction value (dh /
dt) ′, while plastic deformation is dominant in the temperature region Y
Then, correction of the sample volume V → the sample volume correction value V ′ is performed for the GENT equation.

According to the present invention, by such a series of operations, the "viscosity-temperature curve" of the inorganic powder used for the ceramic multilayer substrate, the thick film material and the like can be measured with high accuracy, and the amorphous glass can be used. First, it becomes possible to evaluate the viscosity of a green compact having a viscous behavior very close to the powder state of crystallized glass, glass ceramic composite material and the like.

That is, according to the method for measuring the viscosity of a green compact of the present invention, the viscosity η of a green compact obtained by press-molding an inorganic powder is determined by the GENT equation: η = 2πMGH ⁵ / 3V (dh / dt) ( 2πH ³ + V) (However, M: load, H: sample height, G: gravitational acceleration,
V: sample volume, dh / dt: sample deformation rate), which is a method for measuring the viscosity of a green compact,
(A) a step of obtaining a sample volume correction value V 'of the green compact (where the sample volume correction value V' is the volume occupied by the inorganic powder in the green compact); and (B) a green compact. Step of obtaining a sample deformation speed correction value (dh / dt) 'of the body (where the sample deformation speed correction value (dh / dt)' is the difference between the apparent sample deformation speed and the sample deformation speed due to sintering shrinkage). (C) separating a temperature region X where sintering shrinkage is dominant and a temperature region Y where plastic deformation is dominant with respect to the displacement of the green compact, and (D) a temperature where the sintering shrinkage is dominant. For the region X, the sample volume correction value V ′ is applied as the sample volume V of the GENT formula, and the sample deformation speed correction value (dh / d) is used as the sample deformation speed dh / dt.
(E) applying the sample volume correction value V 'as the sample volume V of the GENT equation for the temperature region Y in which the plastic deformation is dominant;
It has.

In the method for measuring the viscosity of a green compact according to the present invention, a load A
The sample deformation speed (dh / dt) _{A at} , and the sample deformation speed (dh / dt) _B at load _B are determined (however, the load A
≠ Load B), Sample deformation rate under the load A (dh / d
t) _A, performs linear approximation of the sample deformation rate (dh / dt) _B at the load B, obtains the extrapolated value of zero load as a sample deformation rate (dh / dt) ₀ at zero load, the zero load The sample deformation rate (dh / dt) ₀ at is regarded as the sample deformation rate due to the sintering shrinkage, and the sample deformation rate (dh / dt) _A at the load _A or the sample deformation rate at the load B ( A value obtained by subtracting the sample deformation speed (dh / dt) ₀ at zero load from dh / dt) _B can be used as the sample deformation speed correction value (dh / dt) ′.

However, from the sample deformation speed at three or more different loads (for example, load A, load B and load C: where load A ≠ load B ≠ load C), the sample deformation speed at zero load (dh) / Dt) It is desirable to obtain ₀ by linear approximation. The sample deformation rate at zero load (dh / d
This is because t) ₀ can be extracted more accurately.

In this case, in particular, the load A and the load B
Is the load A <load B, and the difference between the sample deformation speed (dh / dt) _B at load _B and the sample deformation speed (dh / dt) ₀ at zero load is the sample deformation speed correction value. (D
h / dt) ′. If the apparent sample deformation speed at the time of calculating the sample deformation speed correction value (dh / dt) ′ is the sample deformation speed when the load is small, the variation in extracting the sample deformation speed correction value tends to increase. There is.

In the method of measuring the viscosity of a green compact according to the present invention, the sample deformation rate (dh / d
t) A sample deformation speed-temperature curve at zero load is prepared according to ₀ , and a minimum value thereof is defined as a boundary temperature Tb. The higher temperature side than Tb can be set as the temperature region Y where the plastic deformation is dominant.

However, the method of extracting the boundary temperature is not limited to the above method. For example, a sample deformation speed-temperature curve for a bulk sample is prepared, and the sample deformation speed-temperature curve at zero load is obtained. The temperature region following the sample deformation speed-temperature curve of the bulk sample can be regarded as a temperature region Y in which plastic deformation is dominant.

Further, in the method of measuring the viscosity of a green compact according to the present invention, the apparent sample deformation speed, ie, the sample deformation speed (dh / dt) _{A under} the load _A , and the sample deformation speed (D) under the load B ( dh / dt) _B can be measured by a parallel plate pressure viscometer. A similar parallel plate pressure viscometer can be used when measuring the sample deformation rate for three or more different loads. As shown in FIG. 15, the parallel plate pressure viscometer sandwiches the object to be measured (compact molded body) between the parallel plates and raises the temperature while applying a constant load, thereby obtaining a sample of the object to be measured. This is a device that detects the deformation speed.

In the method for measuring the viscosity of a green compact according to the present invention, a crystallized glass powder,
One kind of oxide inorganic powder selected from the group consisting of amorphous glass powder and glass-ceramic composite powder can be used. By measuring the viscosities of these powders, it is possible to accurately grasp the viscosity parameters that control and control the characteristics of the ceramic multilayer substrate and the thick film material.

The present invention is not limited to the measurement of the viscosity of a green compact formed by press-molding these oxide inorganic powders. For example, oxide ceramic powder, non-oxide ceramic powder It can also be applied to the viscosity measurement.

Next, an apparatus for measuring the viscosity of a green compact according to the present invention will be described.

The apparatus for measuring the viscosity of a green compact according to the present invention measures the viscosity η of a green compact obtained by press-molding an inorganic powder.
ENT formula: η = 2πMGH ⁵ / 3V (dh / dt) (2πH ³ + V) (However, M: load, H: sample height, G: gravity acceleration,
V: a sample volume, dh / dt: sample deformation rate), which is a device for measuring the viscosity of a green compact,
(A) a sample shape measuring unit for measuring an actual measured value of the shape of the green compact; (b) a sample deformation speed measuring unit for measuring an apparent sample deformation speed of the green compact; (c) the green compacting Based on the measured shape of the body, the volume occupied by the inorganic powder in the green compact is calculated, and this is calculated as a sample volume correction value V ′.
(D) calculating the difference between the apparent sample deformation speed and the sample deformation speed associated with the sintering shrinkage of the green compact, and correcting the sample deformation speed of the green compact ( dh / dt) ′, and (e) formulating a boundary temperature between a temperature region X in which sintering shrinkage is dominant and a temperature region Y in which plastic deformation is dominant with respect to the displacement of the green compact. (F) For the temperature region X in which the sintering shrinkage is dominant, the sample volume correction value V ′ is applied as the sample volume V of the GENT equation, and the sample deformation speed dh / dt is set as the sample deformation speed dh / dt. Sample deformation speed correction value (dh / d
t) ′, an arithmetic processing means for outputting the viscosity η in the temperature region X, (g) in the temperature region Y where the plastic deformation is dominant, the sample volume V of the GENT equation is used as the sample volume Arithmetic processing means for outputting the viscosity η in the temperature region Y by applying the correction value V ′; (h) a display unit for displaying the viscosity η in the temperature region X and the viscosity η in the temperature region Y; It is provided with.

In the apparatus for measuring the viscosity of a green compact according to the present invention, the apparent sample deformation rate is a sample deformation rate (dh / dt) _{A under} a load _A , and a sample deformation rate (dh / dt) under a load B. ) A sample deformation speed measurement unit (where load A ≠ load B) that outputs _B respectively, a sample deformation speed (dh / dt) _A under the load A, and a sample deformation speed (dh / dt) B under the load _B Is a value extrapolated to zero load, that is, the sample deformation rate at zero load (dh / d
t) _0, which outputs the sample deformation speed at the load A (dh / dt), considering the sample deformation speed at zero load (dh / dt) ₀ as the sample deformation speed accompanying the sintering shrinkage.
dt) _A or the sample deformation rate at the load B (dh /
dt) From _B , the sample deformation rate at the zero load (dh /
dt) It is preferable that the apparatus further comprises arithmetic processing means for outputting a value obtained by subtracting ₀ as the sample deformation speed correction value (dh / dt) ′.

Further, the apparatus for measuring the viscosity of a green compact according to the present invention determines the relationship between the load A and the load B by the following equation: load A <load B
The difference between the sample deformation speed at load B (dh / dt) _B and the sample deformation speed at zero load (dh / dt) ₀ is output as the sample deformation speed correction value (dh / dt) ′. It is desirable to provide arithmetic processing means for performing the above.

The apparatus for measuring the viscosity of a green compact according to the present invention produces a sample deformation speed at zero load-temperature curve according to the sample deformation speed at zero load (dh / dt) ₀ , With the value as the boundary temperature Tb, a calculation process for extracting a temperature lower than the boundary temperature Tb as a temperature region X in which the sintering shrinkage is dominant and extracting a temperature higher than the boundary temperature Tb as a temperature region Y in which the plastic deformation is dominant It is desirable to have means.

Further, in the apparatus for measuring the viscosity of a green compact according to the present invention, the sample deformation speed measuring section for actually measuring the apparent sample deformation speed includes, for example, a parallel plate pressure viscometer as shown in FIG. Is desirable.

Further, it is preferable that the apparatus for measuring the viscosity of a green compact according to the present invention comprises a computer having each of the above-mentioned arithmetic processing means. That is, if a computer having a program for executing the above-described series of arithmetic processing is used, the viscosity η of the green compact is measured simply by inputting the sample shape, the sample deformation speed, and the like.

Next, an outline of the apparatus for measuring the viscosity of a green compact according to the present invention will be described with reference to FIG.

The apparatus for measuring the viscosity of a green compact shown in FIG. 7 uses a sample shape measuring section (a sample shape measuring section (height, volume, filling rate, etc.) of a green compact to measure actual measured values. a), a sample deformation speed measuring unit (b) for actually measuring an apparent sample deformation speed with respect to a plurality of loads, and based on actual measurement data from the sample shape measuring unit, the inorganic powder in the green compact is formed. An arithmetic processing means (c) for calculating the occupied volume and outputting this as a sample volume correction value V ', an apparent sample deformation speed based on a measurement value from a sample deformation speed measurement unit, and sintering shrinkage of the green compact; The difference in sample deformation speed due to the above is calculated, and the sample deformation speed correction value (dh / d
calculation processing means (d) for outputting t) ′, calculation processing for determining the boundary temperature Tb of the temperature region X where sintering shrinkage is dominant and the temperature region Y where plastic deformation is dominant for the displacement of the green compact. Means (e), for the temperature region X in which sintering shrinkage is dominant, the sample volume correction value V ′ is defined as the sample volume V in the GENT formula.
And applying the sample deformation speed correction value (dh / dt) ′ as the sample deformation speed dh / dt,
Arithmetic processing means (f) for outputting the viscosity η in the temperature region X;
An arithmetic processing unit (g) for outputting the viscosity η in the temperature region Y by applying the sample volume correction value V ′ as the sample volume V in the GENT equation for the temperature region Y where plastic deformation is dominant. A display unit (h) for displaying the viscosity η in the temperature region X and the viscosity η in the temperature region Y.

Next, a specific application example of this device will be described with reference to FIG.

First, as shown in FIG. 8, in the sample shape measuring section 10, the height (sample height), volume (sample volume), weight (sample weight), weight of inorganic powder, The specific gravity, the amount of the mixture, and the amount of the vehicle such as the binder and the solvent are accurately measured by a pycnometer, an electronic balance, or the like.

On the other hand, in the sample deformation speed measuring section 11,
Actually measured sample deformation rate at a load _A (dh / dt) A, sample deformation rate of a load B a (dh / dt) _B, respectively. In the case of a sample deformation rate measuring unit provided with a parallel plate pressure viscometer, temperature data and sample height data over time are output from the parallel plate pressure viscometer, and by processing these data, dh / dt) _A and (dh / dt) _B are calculated. Further, based on the actually measured data, the sample deformation rate at the load A-temperature curve ｛(dh / dt) _A −
A T curve｝ and a sample deformation rate-temperature curve under load B {(dh / dt) _B -T curve} are simultaneously produced.

Next, the arithmetic processing means 12 calculates the volume occupied by the inorganic powder in the green compact based on the actually measured data from the sample shape measuring section 10 and outputs this as a sample volume correction value V '.

The arithmetic processing means 13 outputs a sample deformation speed (dh / dt) ₀ at zero load based on the actually measured data (or processed data) output from the sample deformation speed measuring section 11. . Specifically, by performing linear approximation using the least squares method the sample deformation rate at a load _A (dh / dt) A, the sample deformation rate (dh / dt) _B at load B, extrapolated value Output the sample deformation speed (dh / dt) ₀ at zero load.

Then, in the arithmetic processing means 14, the load
Sample deformation speed at A (dh / dt) _AOr the load
Sample deformation speed at B (dh / dt)_BFrom zero load
Sample deformation speed (dh / dt)₀Subtract the value from the sample
It is output as a deformation speed correction value (dh / dt) '.

On the other hand, the arithmetic processing means 15 extracts the minimum value according to the sample deformation speed-temperature curve {(dh / dt) ₀ -T curve} from the arithmetic processing means 13 when the load is zero, and extracts the minimum value. Is determined as the boundary temperature Tb. The lower temperature side of the boundary temperature Tb is defined as a temperature region X in which sintering shrinkage is dominant, and the higher temperature side of the boundary temperature Tb is defined as a temperature region Y in which plastic deformation is dominant. Output each one.

Next, for the temperature region X where sintering shrinkage is dominant, the sample volume correction value V ′,
The sample deformation speed correction value (dh / d
t) ′ are input to the arithmetic processing means 18. On the other hand,
The sample volume correction value V ′ from the arithmetic processing unit 12 is input to the arithmetic processing unit 18 for the temperature region Y in which plastic deformation is dominant.

Next, the arithmetic processing means 18 applies the respective correction values to the GENT equation in the temperature region X where sintering shrinkage is dominant and the temperature region Y where plastic deformation is dominant as described above, and calculates the viscosity η. calculate. Since the data of the sample height H of the green compact is required in the GENT equation, this data is input from the sample shape measuring unit 10 to the arithmetic processing unit 18.

Then, the viscosity η calculated by the arithmetic processing means 18 is displayed on a display unit 19 such as a CRT or LCD. In the display unit 19, the viscosity η at each temperature may be displayed in a table format, or may be displayed as a viscosity-temperature curve.

According to the apparatus for measuring the viscosity of a green compact of the present invention, the "viscosity" of inorganic powder used for a ceramic multilayer substrate or a thick film material can be efficiently measured by the above-described series of operations. In addition to amorphous glass powder, crystallized glass, glass-ceramic composite materials, and the like, it is possible to evaluate the viscosity of a green compact having a viscous behavior very close to the powder state.

The computer-readable recording medium on which the method for measuring the viscosity of the compact of the present invention is recorded is a computer-readable recording medium on which a series of steps in the method for measuring the viscosity of the compact of the present invention described above are recorded. Examples of the recording medium include a recording medium such as a magnetic disk of a computer and a recording medium such as a semiconductor memory, and a recording medium such as a portable magnetic tape, a magnetic disk, and an optical disk.

[0071]

The present invention will be described below with reference to specific examples. Sample preparation was first produced crystallized glass of _{SiO 2 -B 2 O 3 -Al 2} O 3 -CaO based. Table 2 below shows the composition system, powder characteristics, and the like of this glass.

[0072]

[Table 2]

Next, an organic vehicle such as toluene or echinene was added to the crystallized glass powder having the composition shown in Table 2 and mixed and dispersed using a ball mill. Thereafter, this is press-formed using a press die (φ7 mm), and a height of 8 to
Columnar compacts having a diameter of 8.5 mm and a diameter of 7 to 7.5 mm (samples A, B, and C) were prepared. And about Sample A, Sample B, and Sample C, the diameter and height were measured with a micrometer, and the sample weight was measured with the electronic balance. Table 3 below shows the measurement results of the sample shapes.

[0074]

[Table 3]

For comparison, a bulk sample was prepared using a glass powder having the composition shown in Table 2. This bulk sample was prepared by placing glass powder in a platinum crucible at a melting temperature of 165.
After pouring at 0 ° C. and gradually cooling from 650 ° C. to room temperature, the sample was polished with a polishing apparatus to obtain parallelism. The obtained sample is a cylindrical bulk sample having a height of 6 mm and a diameter of 7 mm. Sample Volume Correction Next, the sample volume correction values V ′ of the samples A, B, and C were calculated. The sample volume correction value V ′ is a value obtained by multiplying the apparent volume V of each sample by the filling rate of the crystallized glass powder. The results of the sample volume correction are shown in Table 4 below.

[0076]

[Table 4]

Correction of Sample Deformation Speed and Extraction of Boundary Temperature Next, for a green compact (sample A, sample B, sample C), a glass parallel plate pressure viscometer (manufactured by Opto Corporation) having the structure shown in FIG. Was used to measure the sample deformation rate. For sample A, load 56.8 g; for sample B, load 1
A load of 408.8 g was applied to 38.8 g of Sample C, and the rate of temperature rise of the parallel plate pressure viscometer was 5 ° C./min. Similarly, the sample deformation rate of the bulk sample was measured (load: 138.8 g). FIG. 9 shows the measurement results of the sample deformation speed at each temperature.

Sample A (load: 56.8 g), Sample B
As shown in FIG. 4, a value extrapolated to zero load by a linear approximation by the least squares method, ie, a sample deformation rate at zero load (load: 138.8 g) and sample C (load: 408.8 g) ( dh / dt) ₀ was calculated. FIG. 9 also shows the sample deformation rate (dh / dt) ₀ at zero load at each temperature.

As shown in FIG. 9, the sample deformation rate (dh / dt) ₀ at zero load and the sample deformation rate of the bulk sample have a large difference up to around 760 ° C. From around ℃ to around 830 ° C, the sample deformation rates of both samples are almost the same. The reason why the two do not coincide with each other at about 830 ° C. or higher is that the green compact is crystallized and the sample deformation speed at zero load does not follow the sample deformation speed of the bulk sample.

From this, it is considered that the temperature range X up to 760 ° C. is where the sintering shrinkage is dominant. Therefore,
The sample deformation speed (dh / dt) ₀ at zero load may be regarded as the deformation speed accompanying sintering shrinkage. Therefore, in the region up to 760 ° C., the sample deformation rate (dh / dh) at zero load is determined from the measured value of the apparent sample deformation rate of the green compact (that is, the sample deformation rate of sample A, sample B or sample C). dt) The value obtained by subtracting ₀ is defined as a sample deformation speed correction value V ′.

In addition, the higher the load, the greater the effect of viscous flow on the sample deformation rate and the smaller the effect of the load on sintering shrinkage.
The value obtained by subtracting the sample deformation speed at zero load from the sample deformation speed of 08.8 g) is the sample deformation speed correction value (dh / d).
t) ′.

When the temperature is 760 ° C. or higher (up to 830 ° C.),
The sample deformation speed (dh / dt) ₀ at zero load is close to the sample deformation speed of the bulk sample, and it is considered that the plastic deformation due to viscous flow is the dominant temperature region. However, as can be seen from FIG. 9, as the load is increased, the sample deformation speed-temperature curve shifts to a lower temperature side (when the load is 56.8 g, the behavior is almost the same as when the load is zero). This suggests that when the load is increased, sample deformation is added to the plastic deformation due to the effect of the load (= the effect of promoting the sintering by the load). However, the load is taken into account by the GENT formula, and this effect is considered. Is considered to be reflected on the viscosity value.

Therefore, here, the boundary temperature is set to 760 ° C., and the temperature range X where the sintering shrinkage is dominant on the side lower than 760 ° C. and the temperature range Y where the plastic deformation is dominant on the side higher than 760 ° C. . Note that the minimum value of the sample deformation speed-temperature curve at zero load shown in FIG. 9 matches this boundary temperature, and the minimum value of the sample deformation speed-temperature curve at zero load is that the sintering shrinkage is small. It can be seen that the dominant temperature region X and the plastic deformation correspond to the boundary temperature of the dominant temperature region Y. Calculation of Viscosity (Application to GENT Equation) Next, the sample volume correction value V ′ and the sample deformation speed correction value (dh / dt) ′ obtained as described above are applied to the GENT equation, and the viscosity of each sample is calculated. Measure. That is, in the temperature region X where sintering shrinkage is dominant, the sample volume correction value V ′ is applied as the sample volume V of the GENT equation, and the sample deformation speed dh
The sample deformation speed correction value (dh / dt) 'is applied as / dt. In the temperature region Y where plastic deformation is dominant, G
The sample volume correction value V ′ is applied as the sample volume V of the ENT formula.

The viscosity-temperature curves prepared according to the GENT equation are shown in FIGS. Sample A (load 56.8
FIG. 10 shows the viscosity-temperature curve for g), FIG. 11 shows the viscosity-temperature curve for sample B (load 138.8 g), and FIG. 12 shows the viscosity-temperature curve for sample C (load 408.8 g). .

Sample A (load: 56.8 g), Sample B
(Load 138.8 g) and sample C (load 408.8 g), temperature region X where sintering shrinkage is dominant, temperature region Y where plastic deformation is dominant, raw data values (GEN without correction)
Table 5 below shows the relationship between the viscosity and the viscosity of the bulk sample (value when applied to the T formula).

[0086]

[Table 5]

As can be seen from FIGS. 10 to 12 and Table 5,
In the temperature region X where sintering shrinkage is dominant, the sample volume correction value V ′ is applied as the sample volume V in the GENT equation, and the sample deformation speed correction value (dh / dt) is used as the sample deformation speed dh / dt.
dt) ′, and in the temperature region Y where plastic deformation is dominant, by applying the sample volume correction value V ′ as the sample volume V of the GENT equation, the deviation from the viscosity measurement result in the bulk sample is obtained. Could be approached to about 5 ° C. to 10 ° C. If the handling of the sample volume (initial value) and other error factors are further corrected, the viscosity behavior can be made closer to that of the bulk sample.

As can be seen from FIGS. 10 to 12 and Table 5, it was found that the bulk sample did not show an increase in viscosity due to crystallization seen in the compact. The increase in the viscosity of the green compact was determined by the DS in FIGS. 13 and 14.
As shown in the analysis result by C, it almost coincided with the crystallization start temperature Tc.

As described above, by performing the following corrections to the GENT formula, the viscosity measurement of the compact was able to be performed with high precision and efficiency. (1) Regarding the displacement of the green compact, a temperature region X in which sintering shrinkage is dominant and a temperature region Y in which plastic deformation is dominant are separated.
In other words, the separation between the deformation speed associated with sintering shrinkage and the deformation speed associated with plastic deformation included in the sample deformation speed (measured value). (2) In the temperature region X where sintering shrinkage is dominant, sample volume correction and sample deformation speed correction are performed. (3) In the temperature region Y where plastic deformation is dominant, sample volume correction is performed.

[0090]

According to the method for measuring the viscosity of a green compact according to the present invention, a green compact formed by press-molding an inorganic powder such as a crystallized glass powder, an amorphous glass powder or a glass-ceramic composite powder can be obtained. Since the viscosity is measured according to the above-described steps, the viscosity behavior of the green compact is evaluated with high accuracy, particularly in the medium viscosity range of 10 ⁴ to 10 ⁹ Pa · S, which is extremely important in the sintering process and the like. Can be measured.

According to the apparatus for measuring the viscosity of a green compact according to the present invention, the viscosity of a green compact obtained by press-molding an inorganic powder is measured using the above-described sample shape measuring section, sample deformation rate measuring section, and various arithmetic processing. Since the means is provided, the viscous behavior of the green compact can be measured efficiently.

The computer-readable recording medium on which the method for measuring the viscosity of the green compact according to the present invention is a computer-readable recording medium on which the method for measuring the viscosity of the green compact according to the present invention is described. Thereby, the method for measuring the viscosity of the green compact of the present invention can be stored, and the technology can be easily transferred.
Many people can use it easily.

[Brief description of the drawings]

FIG. 1 is a viscosity-temperature curve showing the difference in the viscosity behavior between a green compact and a bulk sample.

FIG. 2 shows a method for measuring the viscosity of a green compact according to the present invention.
5 is a flowchart for explaining a step of extracting a sample volume correction value.

FIG. 3 shows a method for measuring the viscosity of a green compact according to the present invention.
5 is a sample deformation speed-temperature curve for conceptually explaining sample deformation speed correction.

FIG. 4 shows a method for measuring the viscosity of a green compact according to the present invention.
5 is a flowchart for explaining a step of extracting a sample deformation speed correction value and a step of determining a boundary temperature between a temperature region in which sintering shrinkage is dominant and a temperature region in which plastic deformation is dominant.

FIG. 5 shows a method for measuring the viscosity of a green compact according to the present invention.
Sample deformation rate to explain the boundary temperature between the temperature region where sintering shrinkage is dominant and the temperature region where plastic deformation is dominant-
It is a temperature curve.

FIG. 6 shows a method for measuring the viscosity of a green compact according to the present invention.
9 is a flowchart for explaining a method of applying a sample volume correction value and a sample deformation speed correction value to a GENT formula.

FIG. 7 is a schematic flow chart of the apparatus for measuring the viscosity of a green compact of the present invention.

FIG. 8 is a block diagram showing a specific application example of the viscosity measuring device for a green compact according to the present invention.

FIG. 9 is a sample deformation speed-temperature curve showing a difference in sample deformation speed due to a load in the example of the present invention.

FIG. 10 shows a sample A (with a load of 56.8) according to an embodiment of the present invention.
g) is a viscosity-temperature curve.

FIG. 11 shows a sample B (load 138. load) according to an embodiment of the present invention.
8g) is a viscosity-temperature curve.

FIG. 12 shows a sample C (with a load of 408.C.) according to the embodiment of the present invention.
8g) is a viscosity-temperature curve.

FIG. 13 is a graph showing a DSC analysis result of a green compact according to an example of the present invention.

FIG. 14 is a graph showing a DSC analysis result of a bulk sample according to an example of the present invention.

FIG. 15 is a schematic sectional view of a parallel plate pressure viscometer.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 ... Measurement object 2a, 2b ... Quartz plate 3 ... Support base 4 ... Quartz rod 5 ... Heater 6 ... Device

──────────────────────────────────────────────────続 き Continuation of the front page (58) Field surveyed (Int. Cl. ⁷ , DB name) G01N 11/00-11/16 G01N 3/00 JICST file (JOIS)

Claims (13)

(57) [Claims] 1. The viscosity η of a green compact formed by press-molding an inorganic powder is determined by the GENT formula: η = 2πMGH ⁵ / 3V (dh / dt) (2πH ³ + V) (where M: load, H: Sample height, G: gravitational acceleration,
V: sample volume, dh / dt: sample deformation rate), which is a method for measuring the viscosity of a green compact,
(A) a step of determining a sample volume correction value V ′ of the green compact (where the sample volume correction value V ′ is the volume occupied by the inorganic powder in the green compact); The sample deformation speed correction value (dh / dt) 'of the molded body (where the sample deformation speed correction value (dh / dt)' is the difference between the apparent sample deformation speed and the sample deformation speed due to sintering shrinkage) is determined. (C) separating a temperature region X where sintering shrinkage is dominant and a temperature region Y where plastic deformation is dominant with respect to the displacement of the green compact, and (D) the sintering shrinkage is dominant. For the temperature region X, the sample volume correction value V ′ is applied as the sample volume V of the GENT equation, and the sample deformation speed correction value (dh / dh) is used as the sample deformation speed dh / dt.
dt) ′, and (E) applying the sample volume correction value V ′ as the sample volume V of the GENT equation for the temperature region Y where the plastic deformation is dominant. A method for measuring the viscosity of a green compact. Wherein the sample deformation rate of the apparent determined sample deformation rate (dh / dt) _A at load A, the sample deformation rate under a load B a (dh / dt) _B respectively (where load A ≠ load B), the sample deformation rate under the load A (dh / d
t) _A , Sample deformation speed at load B (dh / dt) By linear approximation of _B , sample deformation speed at zero load (dh / dt)
dt) ₀ is determined, and the sample deformation speed at the load of zero (dh / dt) ₀ is regarded as the sample deformation speed accompanying the sintering shrinkage, and the sample deformation speed at the load A (dh / dt) _A or from the sample deformation rate (dh / dt) _B at the load B, and the value obtained by subtracting the sample deformation rate (dh / dt) ₀ at the zero load, and the sample deformation rate correction value (dh / dt) ' The method for measuring the viscosity of a green compact according to claim 1, wherein: 3. The relationship between the load A and the load B is defined as load A <load B, and the sample deformation speed (dh / d
t) _B and the sample deformation rate at the zero load (dh / d)
t) The difference from ₀ is calculated as the sample deformation speed correction value (dh / d
The method for measuring the viscosity of a green compact according to claim 1, wherein t) ′. 4. The sample deformation rate at zero load (dh /
dt) A sample deformation speed-temperature curve at zero load is prepared according to ₀ , and a minimum value thereof is defined as a boundary temperature Tb. The method for measuring the viscosity of a green compact according to any one of claims 1 to 3, wherein a higher temperature side than Tb is defined as a temperature region Y in which the plastic deformation is dominant. 5. The method of measuring the viscosity of a green compact according to claim 1, wherein the apparent deformation rate of the sample is measured by a parallel plate pressure viscometer. 6. The method according to claim 1, wherein the inorganic powder is one kind of oxide inorganic powder selected from the group consisting of crystallized glass powder, amorphous glass powder, and glass-ceramic composite powder. 6. The method for measuring the viscosity of a green compact according to any one of 1 to 5. 7. The viscosity η of a green compact formed by press-molding an inorganic powder is determined by the GENT formula: η = 2πMGH ⁵ / 3V (dh / dt) (2πH ³ + V) (where M: load, H: Sample height, G: gravitational acceleration,
V: a sample volume, dh / dt: sample deformation rate), which is a device for measuring the viscosity of a green compact,
(A) a sample shape measuring unit for measuring an actual measured value of the shape of the green compact; (b) a sample deformation speed measuring unit for measuring an apparent sample deformation speed of the green compact; (c) the green compacting Based on the measured shape of the body, the volume occupied by the inorganic powder in the green compact is calculated, and this is calculated as a sample volume correction value V ′.
(D) calculating the difference between the apparent sample deformation speed and the sample deformation speed associated with the sintering shrinkage of the green compact, and correcting the sample deformation speed of the green compact ( dh / dt) ′, and (e) formulating a boundary temperature between a temperature region X in which sintering shrinkage is dominant and a temperature region Y in which plastic deformation is dominant with respect to the displacement of the green compact. (F) For the temperature region X in which the sintering shrinkage is dominant, the sample volume correction value V ′ is applied as the sample volume V of the GENT equation, and the sample deformation speed dh / dt is set as the sample deformation speed dh / dt. Sample deformation speed correction value (dh / d
t) ′, a processing means for outputting the viscosity η in the temperature region X, (g) in the temperature region Y where the plastic deformation is dominant, the sample volume V of the GENT formula is used as the sample volume Arithmetic processing means for outputting the viscosity η in the temperature region Y by applying the correction value V ′; (h) a display unit for displaying the viscosity η in the temperature region X and the viscosity η in the temperature region Y; A device for measuring the viscosity of a green compact, comprising: 8. As a sample deformation rate of the apparent sample deformation rate at a load _A (dh / dt) A, the sample deformation rate (dh / dt) sample deformation rate measuring unit for outputting _B each with a load B ( However, the load a ≠ load B), the load sample deformation rate (dh / dt in a) _a, by the sample deformation rate (linear approximation of dh / dt) _B at the load B, extrapolated to zero load value , i.e. the arithmetic processing means for outputting a sample deformation rate (dh / dt) ₀ at zero load, the sample deformation rate (dh / dt) ₀ at the zero load regarded as a sample deformation rate caused by the sintering shrinkage, the A value obtained by subtracting the sample deformation speed (dh / dt) ₀ at the zero load from the sample deformation speed (dh / dt) _A at the load _A or the sample deformation speed (dh / dt) _B at the load _B. With the sample deformation speed correction value (dh / dt) ′ The viscosity measuring device for a green compact according to claim 7, further comprising an arithmetic processing unit that outputs the result. 9. The relationship between the load A and the load B is defined as load A <load B, and the sample deformation speed (dh / d
t) _B and the sample deformation rate at the zero load (dh / d)
t) The difference from ₀ is calculated as the sample deformation speed correction value (dh / d
The device for measuring the viscosity of a green compact according to claim 7, further comprising an arithmetic processing unit that outputs the data as t) ′. 10. The sample deformation speed (dh) at zero load.
/ Dt) A sample deformation speed-temperature curve at zero load is prepared according to ₀ , and a minimum value thereof is defined as a boundary temperature Tb. The viscosity measuring device for a green compact according to any one of claims 7 to 9, further comprising an arithmetic processing unit for extracting a higher temperature side than the temperature Tb as a temperature region Y in which the plastic deformation is dominant. . 11. The green compact according to claim 7, wherein the sample deformation rate measuring unit for measuring the apparent sample deformation rate comprises a parallel plate pressure viscometer. Viscosity measuring device. 12. The apparatus for measuring the viscosity of a green compact according to claim 7, further comprising a computer having said arithmetic processing means. 13. A method for measuring the viscosity of a green compact, characterized by recording a program for causing a computer to execute the method for measuring the viscosity of a green compact according to any one of claims 1 to 6. Computer readable recording medium.