CN104458486B - The method of testing of tenor in a kind of diamond dust post - Google Patents
The method of testing of tenor in a kind of diamond dust post Download PDFInfo
- Publication number
- CN104458486B CN104458486B CN201410758993.9A CN201410758993A CN104458486B CN 104458486 B CN104458486 B CN 104458486B CN 201410758993 A CN201410758993 A CN 201410758993A CN 104458486 B CN104458486 B CN 104458486B
- Authority
- CN
- China
- Prior art keywords
- crucible
- stove
- sample
- tenor
- burning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses the method for testing of tenor in a kind of diamond dust post, prepared by its step: A, sample: by sample sawing or grind to form fine powder；B, pre-burning crucible: a planar shaped ceramic crucible lid is cleaned up, pre-burning in stove；C, charging: after crucible naturally cools to room temperature in exsiccator, weigh as G2；D, take fine powder sample, add pre-burning crucible, uniformly pave, weigh as G2+G；Stove calcination put into by E, the crucible that will be equipped with sample；F, come out of the stove after natural cooling, place into and exsiccator be cooled to room temperature, be then charged into vacuum sintering furnace, evacuation is discharged, then is passed through hydrogen and reduces, deoxidation；G, cooling are come out of the stove to room temperature, weigh as G1.Easy to implement the method, equipment is simple, easy to operate, provides quickly in high-volume diamond dust post production process, convenient, test result accurately, it is adaptable to the mensuration of the tenor of diamond synthesis powder pillar.
Description
Technical field
The present invention relates to China superhard material Industry technical field, be more particularly to tenor in a kind of diamond dust post
Method of testing, can be widely applied to the mensuration of tenor in diamond dust post, especially raw at high-volume diamond dust post
It is convenient to provide during product, test result accurately.
Background technology
Diamond synthesis powder pillar is mainly made up of carbon source material and metal solvent material, the examination of its tenor,
In general, it is all the physicochemical analysis test method according to national Specification, it is possible to use the scanning of х fluorescence spectrophotometer
Carry out, or select carbon and sulfur analytical instrument to test.But, its content of graphite diamond more than 60% powder pillar is come
Saying, also should not test with carbon and sulfur analytical instrument, this analysis test method is to utilize diamond powder pillar in vacuum-sintering operation
In, existing high-temperature hydrogen reduction condition, use the method for " powder process is weighed-oxidation-reduction-weigh " to realize, have
Method is easy, and test funds are cheap, feature fast and accurately, according to the method for х fluorescence spectrophotometer scanning, invest an instrument
Device just needs hundreds of thousands, very causes unit up to a million, and testing expense is the highest.
Summary of the invention
It is an object of the invention to there are provided the method for testing of tenor in a kind of diamond dust post, use system
Powder, weigh, aoxidize de-carbon, reduction deoxidation, the method weighed realize, the method has easy and simple to handle, quickly, accurately, test
Expense is few, feature with low cost.
In order to realize above-mentioned purpose, the present invention uses techniques below measure:
In a kind of diamond dust post, the method for testing of tenor, comprises the following steps:
1, prepared by sample: by sample sawing or grind to form thin 24-26 mesh powder, weighs with ten thousand/precision analysis balance
2～3g.
2, pre-burning crucible: a planar shaped ceramic crucible lid is cleaned up, pre-burning 50 to 60 in the stove of 900-915 DEG C
Minute.
3, charging: after crucible naturally cools to room temperature (15-25 DEG C, the most identical) in exsiccator, weigh as G2 (little
Type ceramic crucible, about 30g).
4, take 2～3g fine powder samples, add pre-burning crucible, uniformly pave, weigh into G2+G (crucible and sample, about
32.5g)。
5, will be equipped with the crucible of sample and put into the stove calcination 20 of 900-915 DEG C～22 hours.
6, natural cooling (temperature is less than 200 DEG C) 5 to 6 minutes after coming out of the stove, (temperature is 35-to place into cooling in exsiccator
40 DEG C) to room temperature, it is then charged into vacuum sintering furnace (VHS-30 type), in the stove of 1105-1115 DEG C, being passed through purity is
The nitrogen of 99.99%, after maintaining 8-12 minute, evacuation is discharged, then is passed through hydrogen and reduces, deoxidation.
7, cooling (temperature is 35-40 DEG C) is come out of the stove to room temperature, weighs as G1, obtains metal accurately by calculating and contain
Amount, computing formula:
Tenor=(G1-G2) ÷ G × 100%
In formula: G=(G2+G)-G2
The weight () of G2--pre-burning crucible
The weight () of G--test specimens
G1--the crucible after reduction and the weight () of sample.
The present invention compared with prior art, has the following advantages and effect:
The technique effect of this technical scheme and the effectiveness comparison of prior art: with compared with X fluorescence spectrometer test, can drop
Low testing expense more than 60%, test result is more directly perceived, accurately.Easy to implement the method, equipment is simple, easy to operate, in high-volume
Diamond dust post production process provides quickly, convenient, test result accurately, tenor be 29.50%～
30.50%.By test, metal result content is respectively as follows: 29.82%；29.93%；29.78%；29.85%；30.29%；
30.31%.
Accompanying drawing explanation
Fig. 1 is the method for testing schematic diagram of tenor in a kind of diamond dust post.
Detailed description of the invention
Embodiment 1:
In a kind of diamond dust post, the method for testing of tenor, comprises the following steps:
1, prepared by sample: by sample sawing or grind to form fine powder: 24 or 25 or 26 mesh, with ten thousand/precision analysis sky
Put down and weigh 2 or 3g.
2, pre-burning crucible: a planar shaped ceramic crucible lid is cleaned up, in 905 or 908 or 910 or 912 or 915 DEG C
Pre-burning 50 or 53 or 56 or 58 or 60 minutes in stove.
3, charging: after crucible naturally cools to room temperature (15 or 17 or 19 or 21 or 23 or 25 DEG C) in exsiccator, weighs
For G2 (weight is 18.3325g).
4, take 2 or 3g fine powder samples, add pre-burning crucible, uniformly pave, weigh as G2+G (weight is 2.6865g).
5, the stove calcination 20 or 21 of 905 or 906 or 909 or 911 or 913 or 915 DEG C put into by the crucible that will be equipped with sample
Or 22 hours.
6, after coming out of the stove, natural cooling (temperature is less than 200 DEG C) 5 or 6 minutes, place into and are cooled to room temperature in exsiccator, then
Load vacuum sintering furnace, in the stove of 1105 or 1108 or 1110 or 1113 or 1115 DEG C, be passed through the nitrogen that purity is 99.99%
Gas, after maintaining 8 or 9 or 10 or 11 or 12 minutes, evacuation is discharged, then is passed through hydrogen and reduces, deoxidation.
7, cooling (temperature is 35 or 36 or 37 or 38 or 39 or 40 DEG C) is come out of the stove to room temperature, weighs as G1；
8, computing formula:
Tenor=(G1-G2) ÷ G × 100%
In formula: G=(G2+G)-G2
The weight () of G2--pre-burning crucible
The weight () of G--test specimens
G1--the crucible after reduction and the weight () of sample
Obtaining result by above-mentioned technical measures is: tenor is 29.50%～30.50%, it is adaptable to synthesis gold
The mensuration of the tenor of hard rock powder pillar.By test, concrete outcome is respectively as follows: 29.82%；29.93%；29.78%；
29.85%；30.29%；30.31%.
Claims (1)
1. a method of testing for tenor in diamond dust post, the steps include:
Prepared by A, sample: by sample sawing or grind to form fine powder, weighs 2～3g with ten thousand/precision analysis balance；
B, pre-burning crucible: a planar shaped ceramic crucible lid is cleaned up, pre-burning 50 to 60 minutes in the stove of 900-915 DEG C；
C, charging: after crucible naturally cools to room temperature in exsiccator, weigh as G2；
D, take 2～3g fine powder samples, add pre-burning crucible, uniformly pave, weigh as G2+G；
E, will be equipped with the crucible of sample and put into the stove calcination 20 of 900-915 DEG C～22 hours；
F, come out of the stove after natural cooling 5 to 6 minutes, place into and exsiccator be cooled to room temperature, be then charged into vacuum sintering furnace,
In the stove of 1105-1115 DEG C, being passed through the nitrogen that purity is 99.99%, after maintaining 8-12 minute, evacuation is discharged, then is passed through hydrogen
Gas reduces, deoxidation；
G, cooling are come out of the stove to room temperature, weigh as G1, by calculating acquisition tenor, computing formula:
Tenor=(G1-G2) ÷ G × 100%
In formula: G=(G2+G)-G2
G2--the weight of pre-burning crucible
The weight of G--test specimens
G1--the crucible after reduction and the weight of sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410758993.9A CN104458486B (en) | 2014-12-12 | 2014-12-12 | The method of testing of tenor in a kind of diamond dust post |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410758993.9A CN104458486B (en) | 2014-12-12 | 2014-12-12 | The method of testing of tenor in a kind of diamond dust post |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104458486A CN104458486A (en) | 2015-03-25 |
| CN104458486B true CN104458486B (en) | 2016-09-21 |
Family
ID=52904898
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410758993.9A Active CN104458486B (en) | 2014-12-12 | 2014-12-12 | The method of testing of tenor in a kind of diamond dust post |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104458486B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375640B (en) * | 2018-05-03 | 2021-05-25 | 北京农业质量标准与检测技术研究中心 | Method for extracting form of heavy metal chromium in mushroom based on tube furnace |
| CN113295573B (en) * | 2021-05-21 | 2024-01-16 | 深圳市金质金银珠宝检验研究中心有限公司 | Method for detecting gold content of electroformed hard gold product |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3422032A (en) * | 1965-09-07 | 1969-01-14 | Allied Chem | Synthetic diamantiferous composition |
| EP0491521B1 (en) * | 1990-12-15 | 1997-03-12 | Fujitsu Limited | Process for producing diamond film |
| JP3327080B2 (en) * | 1994-11-30 | 2002-09-24 | 住友電気工業株式会社 | High strength and high wear resistance diamond sintered body and method for producing the same |
| CN102175684B (en) * | 2011-01-07 | 2012-10-10 | 华东师范大学 | Measuring method of glass phase components of alumina ceramic |
| CN102607984A (en) * | 2012-02-29 | 2012-07-25 | 成都中光电科技有限公司 | Test method for compositions of fine silica powder |
-
2014
- 2014-12-12 CN CN201410758993.9A patent/CN104458486B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104458486A (en) | 2015-03-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107340276A (en) | A kind of method of multiple element content in quick measure rare earth metal/alloy | |
| Kostrovitsky et al. | Age of the Siberian craton crust beneath the northern kimberlite fields: Insights to the craton evolution | |
| CN104458486B (en) | The method of testing of tenor in a kind of diamond dust post | |
| CN103063602A (en) | Method for measuring free carbon and silicon carbide in silicon carbide deoxidizing agent | |
| CN103674649A (en) | Preparation method of spectrum standard sample for 1420 aluminum lithium alloy | |
| CN104515766A (en) | Method for measuring impurity elements in graphite slurry | |
| CN113009102A (en) | Method for determining composition of scrap and processing equipment for detecting composition sample of scrap | |
| CN103389232B (en) | The sample preparation methods of X fluorescence spectrum analysed for powder alloy cast iron | |
| CN109557079A (en) | The ICP-OES measuring method of constituent content in sintering dust separation ash | |
| CN102967619B (en) | The method of hydrogen preci-sion and accuracy when raising titanium or the hydrogen translocation of titanium alloy oxygen nitrogen | |
| CN109668871A (en) | The direct-reading spectrometer analysis method of trace amount Ti in a kind of steel | |
| CN113189085A (en) | Method for measuring Mg activity coefficient of Mg-containing blast furnace slag | |
| CN101825588A (en) | Method for measuring contents of As and Sn elements in iron ore by adopting X-ray fluorescence spectrum melting method | |
| JP5214576B2 (en) | Method for measuring the total amount of alkali in hardened concrete | |
| CN112504778B (en) | Energy-containing tungsten alloy standard substance and preparation method thereof | |
| CN101571499B (en) | Method for measuring elements to be measured of samples to be measured | |
| Lim et al. | High-precision analysis of SF 6 at ambient level | |
| CN102175557A (en) | Method for testing trace impurities in ultrahigh-purity graphite | |
| Rondão et al. | A combined structural, microstructural and dilatometric analysis of MgPSZ | |
| RU2488101C1 (en) | Method to detect filler content in polymer composite | |
| Shen et al. | Theoretical analysis of Si3N4/TiC interfacial properties and material preparation | |
| Cetinkol et al. | Scandium tungstate above 2.5 GPa | |
| CN110567944A (en) | Method for measuring trace iron, aluminum, silicon and calcium in vanadium carbide | |
| Ni | Kinetics of the reaction between quartz and silicon carbide in different gas atmospheres | |
| Barrado et al. | Towards the development of technical specifications for the production of lithium–lead alloys for the ITER HCLL TMB |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211011 Address after: No. 188, East Hubei Road, Ezhou, Hubei Province, 436000 Patentee after: Believe diamond new material limited liability company in Hubei Province Address before: 436000 Diamond Industrial Park 188 Edong Avenue, Ezhou City, Hubei Province Patentee before: EZHOU DIAMOND TECHNOLOGY RESEARCH & DEVELOPMENT CENTER |
|
| TR01 | Transfer of patent right |