CN106904983B - A kind of preparation method of the ceramic sample containing Embedded defect - Google Patents
A kind of preparation method of the ceramic sample containing Embedded defect Download PDFInfo
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- CN106904983B CN106904983B CN201710186151.4A CN201710186151A CN106904983B CN 106904983 B CN106904983 B CN 106904983B CN 201710186151 A CN201710186151 A CN 201710186151A CN 106904983 B CN106904983 B CN 106904983B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/74—Ceramic products containing macroscopic reinforcing agents containing shaped metallic materials
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N1/32—Polishing; Etching
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/404—Refractory metals
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Abstract
The invention discloses a kind of preparation method of ceramic sample containing Embedded defect, the first compacting, the addition of high rigidity high melting point metal materials, the secondary compacting of green compact and sintering, the chemistry removals of high rigidity high melting point metal materials, the cleaning of sample of powder green compact are specifically included；By the high rigidity high melting point metal materials that specified size, shape and quantity are added on ceramic green surface, then green compact compacting and sintering, the high rigidity high melting point metal materials on surface are removed finally by the method for chemical attack, to produce the ceramic sample containing Embedded defect.The method of the present invention is simple and practical, can be by selecting have the high rigidity high melting point metal materials of certain shapes and size come the prefabricated ceramic sample containing defect, to consider that System of Detecting Surface Defects For Material provides material preparation technology support to the experimental study of ceramic derogatory behaviour.
Description
Technical field
The present invention relates to the preparations of ceramic material, are specifically related to a kind of preparation method of ceramic sample containing Embedded defect.
Background technique
Ceramic material especially engineering ceramics as a kind of inorganic non-metallic material made through overmolding and high temperature sintering,
The fields such as machinery, microelectronics, aviation are widely used in the advantages that its high-melting-point, high rigidity, high-wearing feature, resistance to oxidation.But
Since ceramics belong to typical hard brittle material, performance is largely influenced by its defect, with fine fisssure in these defects
Line and Micro-v oid are the most typical, therefore it is particularly important to study influence of the defect of ceramic material to its mechanical property.
But numerous scholars are in the experimental study to ceramic material defect, for the ceramic sample containing micro-crack or Micro-v oid
Preparation mostly use artificial scribing greatly, inefficiency and desired effect is bad also will cause other new machining damages, make simultaneously
Standby defect size, shape and depth are all not easy to control.
And the present invention is intended to provide a kind of preparation method of simple and practical, the easy to operate ceramic sample containing Embedded defect,
To consider that System of Detecting Surface Defects For Material provides material preparation technology support to the experimental study of ceramic derogatory behaviour.
Summary of the invention
The present invention is intended to provide a kind of preparation method of simple and practical, the easy to operate ceramic sample containing Embedded defect.It should
Method can artificially make and specify size in ceramic sample, the micro-crack and micropore hole defect of shape and quantity, to consider material table
Planar defect provides material preparation technology support to the experimental study of ceramic derogatory behaviour.
The present invention is achieved by following technical solution.
A kind of preparation method of the ceramic sample containing Embedded defect, the specific steps are as follows:
(1) the first compacting of powder green compact: ready ceramic powder is uniformly poured into compacting tool set and is paved, is then led to
It crosses compacting tool set and ceramic powder is pressed for the first time, control the volume compressibility of powder green compact between 15%-20%；
(2) addition of high rigidity high melting point metal materials: by a certain size, the high rigidity refractory metal of shape and quantity
Material is placed in the upper surface of powder green compact, is uniformly distributed it；
(3) the secondary compacting of green compact and sintering: the powder green compact that step (2) is obtained carry out secondary compacting, cause to be put
The high rigidity high melting point metal materials set are completely embedded into the surface of powder green compact, are then sintered molding；
(4) the chemistry removal of high rigidity high melting point metal materials: the ceramic sample that step (3) is obtained immerses in chloroazotic acid,
Accelerate chemical attack removal efficiency by the method for heating chloroazotic acid, the high rigidity high-melting-point of ceramic sample outer surface after sintering
Metal material all removes；
(5) cleaning of sample finished product: the ceramic sample that step (4) is obtained carries out ultrasonic cleaning, dries, obtains to it
Ceramic sample containing Embedded defect.
Further, the ceramic powder in the step (1) is the ceramic powders of non-metal base.
Further, the high rigidity high melting point metal materials in the step (2) are pure tungsten, and shape is elongated strip
With two kinds of spherical shape, size and quantity can be matched according to the size and density of required Embedded defect.
The beneficial effects of the present invention are: the present invention provides simple and practical, easy to operate ceramic samples containing Embedded defect
Preparation method.This method can artificially make and specify size in ceramic sample, the micro-crack and micropore hole defect of shape and quantity,
To consider that System of Detecting Surface Defects For Material provides material preparation technology support to the experimental study of ceramic derogatory behaviour.
Detailed description of the invention
The present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the process step of the invention schematic diagram.
Fig. 2 is that powder green compact of the invention suppress schematic diagram.
Fig. 3 is process flow chart of the invention.
Specific embodiment
The present invention will be further described below with reference to the drawings.
As shown in Figure 1 to Figure 3, the preparation method of a kind of ceramic sample containing Embedded defect of the invention, the specific steps are as follows:
(1) the first compacting of powder green compact: ready ceramic powder is uniformly poured into compacting tool set and is paved, is then led to
It crosses compacting tool set and ceramic powder is pressed for the first time, control the volume compressibility of powder green compact between 15%-20%；
(2) addition of high rigidity high melting point metal materials: by a certain size, the high rigidity refractory metal of shape and quantity
Material is placed in the upper surface of powder green compact, is uniformly distributed it；
(3) the secondary compacting of green compact and sintering: the powder green compact that step (2) is obtained carry out secondary compacting, cause to be put
The high rigidity high melting point metal materials set are completely embedded into the surface of powder green compact, are then sintered molding；
(4) the chemistry removal of high rigidity high melting point metal materials: the ceramic sample that step (3) is obtained immerses in chloroazotic acid,
Accelerate chemical attack removal efficiency by the method for heating chloroazotic acid, the high rigidity high-melting-point of ceramic sample outer surface after sintering
Metal material all removes；
(5) cleaning of sample finished product: the ceramic sample that step (4) is obtained carries out ultrasonic cleaning, dries, obtains to it
Ceramic sample containing Embedded defect.
Further, the ceramic powder in the step (1) is the ceramic powders of non-metal base.
Further, the high rigidity high melting point metal materials in the step (2) are pure tungsten, and shape is elongated strip
With two kinds of spherical shape, size and quantity can be matched according to the size and density of required Embedded defect.
Embodiment:
Now need the one silicon carbide ceramics sample containing Embedded defect of preparation for experimental study, sample size length is 3cm, high
Degree is 2cm, and width 1cm, Embedded defect includes micro-crack and Micro-v oid, and micro-crack length range is 200 μm -500 μm, width
Range is 15 μm -20 μm, and Micro-v oid diameter range is 50 μm -100 μm, and defect need to be evenly distributed on sample outer surface,
Defect counts are 20.Preparation method is as follows:
(1) ready silicon carbide ceramics powder uniformly the first compacting of powder green compact: is poured into compacting tool set middle berth
It is flat, ceramic powders are pressed by compacting tool set for the first time then, the powder green volume compression ratio to be formed is made to reach 18% left side
The right side, wherein powder volume compressibility=(stacking volume after paving the first pressing of stacking volume-powder of powder)/powder paves heap
Product volume；
(2) addition of high rigidity high melting point metal materials: the high rigidity high-melting-point of the elongated strip of artificial selection and spherical shape
Each 10, metal material tungsten sample, and the number of 1-20 serial number is carried out, wherein elongated strip metal sample length range is 200 μm
- 400 μm, width range is 15 μm -18 μm, and spherical shape metal sample diameter range is 50 μm -80 μm, by its metal material
Material tungsten sample is placed in the upper surface of powder green compact one by one, is uniformly distributed the sample of two kinds of shapes, and recording number is 1-
The placement location of No. 20 metal sample tungsten；
(3) the secondary compacting of green compact and sintering: the powder green compact that step (2) is obtained carry out secondary compacting, cause to be put
The 20 high rigidity refractory metal tungsten samples set are completely embedded into the surface of powder green compact, are seen using ultrasonic scanning microscope
It surveys, the embedded location and effect of tungsten sample after the secondary compression of powder green compact is detected, tungsten sample must not have de-
It falls and raised, is then sintered molding；
(4) the chemistry removal of high rigidity high melting point metal materials: the ceramic sample that step (3) is obtained immerses in chloroazotic acid,
Accelerate chemical attack removal efficiency by the method for heating chloroazotic acid, chemical equation:
With, the high rigidity Gao Rong of ceramic sample outer surface after sintering
Point tungsten all removes；
(5) cleaning of sample finished product: the ceramic sample that step (4) is obtained carries out ultrasonic cleaning, dries to it, then into
The microscopical observation of row ultrasonic scanning, it is ensured that preparation is qualified, then obtains the ceramic sample containing Embedded defect.
Claims (2)
1. a kind of preparation method of ceramic sample containing Embedded defect, it is characterised in that: specific step is as follows:
(1) the first compacting of powder green compact: ready ceramic powder is uniformly poured into compacting tool set and is paved, pressure is then passed through
Molding jig is pressed ceramic powder for the first time, controls the volume compressibility of powder green compact between 15%-20%；The pottery
Ceramic powder is the ceramic powders of non-metal base；
(2) addition of high rigidity high melting point metal materials: by a certain size, the high rigidity high melting point metal materials of shape and quantity
It is placed in the upper surface of powder green compact, is uniformly distributed it；
(3) the secondary compacting of green compact and sintering: the powder green compact that step (2) is obtained carry out secondary compacting, cause to be placed
High rigidity high melting point metal materials are completely embedded into the surface of powder green compact, are then sintered molding；
(4) the chemistry removal of high rigidity high melting point metal materials: the ceramic sample that step (3) is obtained immerses in chloroazotic acid, passes through
The method for heating chloroazotic acid accelerates chemical attack removal efficiency, the high rigidity refractory metal of ceramic sample outer surface after sintering
Material all removes；
(5) cleaning of sample finished product: the ceramic sample that step (4) is obtained carries out ultrasonic cleaning, dries to it, obtains containing pre-
The ceramic sample of defect processed.
2. a kind of preparation method of ceramic sample containing Embedded defect according to claim 1, it is characterised in that: the step
Suddenly the high rigidity high melting point metal materials in (2) are pure tungsten, and shape is elongated strip and two kinds of spherical shape, size sum number
Amount can be matched according to the size and density of required Embedded defect.
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| CN108132169B (en) * | 2017-12-07 | 2020-04-21 | 中国航发动力股份有限公司 | Method for manufacturing laboratory capacity comparison sample |
| CN109030132B (en) * | 2018-06-14 | 2021-02-09 | 国网安徽省电力有限公司电力科学研究院 | Preparation method of creep damage reference block, damage detection method and system |
| CN111238891B (en) * | 2020-01-16 | 2020-11-03 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of internal defects of reaction sintered silicon carbide ceramic |
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| CN103439165B (en) * | 2013-09-11 | 2015-09-30 | 淄博出入境检验检疫局综合技术服务中心 | A kind of preparation method containing cobalt ceramic glaze standard sample |
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